废轮胎热解油的资源化利用研究
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摘要
经济的增长、交通运输业的发达带动了汽车工业的快速发展,随之而来的是废轮胎产生量的不断增加,因此,废轮胎的处理成为国内外专家的研究热点。废轮胎的热解制油技术是目前公认的一条附加值高且环境友好的回收路线,而如何合理利用产生的大量热解油则成为该技术继续发展的关键。本文以工业试验装置生产的废轮胎热解油为研究对象,对其资源化利用进行了研究。主要研究内容如下：
本文在大量文献调查的基础上,首先从热解油的综合分析和评价入手,不仅对热解油,而且还对馏分油、窄馏分油进行了详细分析。结果表明：热解油的金属元素含量低,硫、氮含量高,芳烃含量高；轻、中质馏分的总含量高,其性质和组成分别与FCC(催化裂化)汽、柴油接近；重质馏分的性质和组成与石油沥青相近；并认定了窄馏分油中烃类化合物和非烃类化合物的分布规律；通过对热解油中特殊物质的分析表明,热解油中的酸性化合物主要以脂肪酸的形式存在。
热解油中的轻、中质馏分含量高达62.9%,是热解油资源化利用的重点,而且热解油的性质和组成与石油相似,本文提出利用石油加工手段将热解油加工炼制成石油产品或调合组分,并依据废轮胎热解装置规模小、分散性大的特点,提出将其掺入石油加工装置进行加工的方案。
于是,本文以轻质馏分为典型,对其掺炼至FCC汽油中加氢精制的可行性进行了考察。首先在实验室加氢精制固定床微型反应器上,采用正交实验,考察操作参数(包括掺炼比)对加氢精制过程脱硫率、脱氮率的影响,结果表明反应温度的影响最显著；对轻质馏分掺炼至FCC汽油中进行加氢精制的可行性考察的结果表明：在氢油比512、进油体积空速1.65 h-1、反应温度353℃、反应压力3 MPa、掺量比10%的操作条件下,得到产品的密度、硫含量,以及馏程分布均能达到我国GB/T 17930车用汽油标准；然后,对轻质馏分掺炼至FCC汽油中加氢精制动力学进行了研究,通过对三种模型的筛选,确定了可以用1级加氢精制反应动力学模型来描述HDS、HDN反应,经F统计检验和相对误差信息分析,得到其复相关指数分别为0.9248和0.9794,平均相对误差分别为4.33%和0.87%。
通过对重质馏分的分析,结果表明重质馏分是生产道路沥青的合适原料。于是,本文对重质馏分分别采用蒸馏法、掺入法生产道路沥青的可行性进行了研究。结果表明采用蒸馏法虽然切割温度点在420℃、430℃、440℃的直馏沥青的针入度、软化点、延度均能满足道路沥青的技术指标,但其老化性能无法达标,说明热解油重质馏分采用蒸馏法生产道路沥青不可行；对重质馏分以不同搅拌温度、不同搅拌时间、不同搅拌速率掺入AH-70道路沥青的可行性进行了研究,结果表明在搅拌温度160℃、搅拌时间10 min、搅拌速率2500 r·min-1的条件下,向AH-70道路沥青中掺入1%的重质馏分,可以基本达到AH-70沥青的标准,与此同时其老化后的延展性还能得到很大改善。
以上研究成果,为热解油的资源化利用开辟了一条新的途径,具有重要的学术意义和应用价值。
Large amount of used tires have been produced due to the rapidly growing global economics and automobile industry. To figure out an economic and practical manner on utilization of used tires has come into a stringent task for researches. It is widely known that to pyrolysis used tires is a high value-added and environmentally friendly recycling route. However, the most critical issue during used tires pyrolysis is how to intelligently utilize the specific pyrolysis oil. In this dissertation, used tires pyrolysis oil from industrial unit was used as the starting material. Characterization, utilization and application of used tire pyrolysis oil were studied. The results are expected to provide a principle valuable option for the utilization of used tires. This dissertation mainly consists of the following contents.
A detail analysis and evaluation were conducted on compositions of the used tire pyrolysis oil, including fractions and narrow fractions of the oil. The results showed that pyrolysis oil was low metal content with high sulfur and nitrogen, and high aromatic. The content of light and medium fractions was high up to 62.9% of pyrolysis oil, and the characteristics and compositions were much closed to those of FCC gasoline and FCC (Fluid Catalytic Cracking) diesel, respectively. On the other hand, the characteristics and compositions of heavy fraction were similar to those of petroleum asphalt. The regular pattern of the distribution of hydrocarbon compounds and non-hydrocarbon compounds in narrow fractions were ascertained as well. In the characteristics component analysis of the pyrolysis oil, it was found that the main acidic compounds in the pyrolysis oil were fatty acids which are seldom seen in crude oils.
Pyrolysis oil contained light and medium fractions of 62.9%, which was an important point for utilization of pyrolysis oil. Since the characteristics and compositions of pyrolysis oil were similar to those of crude oil, it is potential to use oil processing methods to process and turn the pyrolysis oil into petroleum products or additive particles. In this dissertation, a distinctive utilization route for the pyrolysis oil was present, which the pyrolysis oil would be incorporated in oil processing plants in consideration of the features of pyrolytic device being small scale and large dispersion.
Light fraction in the pyrolysis oil was used as a model fraction to blend with FCC gasoline, and then the hydrotreating process of the mixture oil was studied. With the method of orthogonal experiment, the hydrotreating operation parameters (including the blending ratio of light fraction to FCC gasoline) on desulphurization and denitrogeneration rate were optimized in the laboratory fixed bed micro-reactor. The results showed that hydrotreating temperature was the most significant factor. Furthermore, the feasibility of hydrotreating of FCC light gasoline blending with light fraction was investigated under industrial operating conditions. The results showed that density, sulfur content and distillation range of the hydrotreating product achieved the standards of gasoline fuels for vehicles under the following conditions:the ratio of hydrogen to oil at 512, the liquid hourly space velocity at 1.65 h-1, reaction temperature at 353℃, reaction pressure at 3 MPa, and blending ratio at 10%. In the three kinetic study models of hydrotreating reaction of FCC gasoline blending with light fraction, the first-order reaction kinetic model was found to describe the HDS and HDN reactions. The analysis of relative error and F statistical analysis showed that the multiple correlation indexes were 0.9248 and 0.9794, and the average relative errors were 4.33% and 0.87%, respectively.
The investigation of heavy fraction composition showed that heavy fraction was potential to produce road asphalt. The feasibility of heavy fraction to produce road asphalt was studied by distillation and blending methods, respectively. The distillation results showed that penetration, softening point, and ductility of straight asphalt of cutting point temperature at 420℃,430℃and 440℃could meet with the major technical index of road asphalt's standards, except for substandard performance after aging. Therefore, heavy fraction producing road asphalt by distillation method was infeasible. On the other hand, under conditions of different mixing temperature, stirring time, stirring speed, and the feasibility of AH-70 road asphalts blending with heavy fraction were discussed. The results showed that the aged ductility of the blending asphalt was greatly enhanced, which can basically match the standard of AH-70 road asphalt. The optimum conditions were mixed at 160℃, stirred at 2500 r-min-1 for 10 min with the blending ratio of 1%.
These results open up a novel route for utilization of used tire pyrolysis oil, and have not only significant academic value but also application value.
本文在大量文献调查的基础上,首先从热解油的综合分析和评价入手,不仅对热解油,而且还对馏分油、窄馏分油进行了详细分析。结果表明：热解油的金属元素含量低,硫、氮含量高,芳烃含量高；轻、中质馏分的总含量高,其性质和组成分别与FCC(催化裂化)汽、柴油接近；重质馏分的性质和组成与石油沥青相近；并认定了窄馏分油中烃类化合物和非烃类化合物的分布规律；通过对热解油中特殊物质的分析表明,热解油中的酸性化合物主要以脂肪酸的形式存在。
热解油中的轻、中质馏分含量高达62.9%,是热解油资源化利用的重点,而且热解油的性质和组成与石油相似,本文提出利用石油加工手段将热解油加工炼制成石油产品或调合组分,并依据废轮胎热解装置规模小、分散性大的特点,提出将其掺入石油加工装置进行加工的方案。
于是,本文以轻质馏分为典型,对其掺炼至FCC汽油中加氢精制的可行性进行了考察。首先在实验室加氢精制固定床微型反应器上,采用正交实验,考察操作参数(包括掺炼比)对加氢精制过程脱硫率、脱氮率的影响,结果表明反应温度的影响最显著；对轻质馏分掺炼至FCC汽油中进行加氢精制的可行性考察的结果表明：在氢油比512、进油体积空速1.65 h-1、反应温度353℃、反应压力3 MPa、掺量比10%的操作条件下,得到产品的密度、硫含量,以及馏程分布均能达到我国GB/T 17930车用汽油标准；然后,对轻质馏分掺炼至FCC汽油中加氢精制动力学进行了研究,通过对三种模型的筛选,确定了可以用1级加氢精制反应动力学模型来描述HDS、HDN反应,经F统计检验和相对误差信息分析,得到其复相关指数分别为0.9248和0.9794,平均相对误差分别为4.33%和0.87%。
通过对重质馏分的分析,结果表明重质馏分是生产道路沥青的合适原料。于是,本文对重质馏分分别采用蒸馏法、掺入法生产道路沥青的可行性进行了研究。结果表明采用蒸馏法虽然切割温度点在420℃、430℃、440℃的直馏沥青的针入度、软化点、延度均能满足道路沥青的技术指标,但其老化性能无法达标,说明热解油重质馏分采用蒸馏法生产道路沥青不可行；对重质馏分以不同搅拌温度、不同搅拌时间、不同搅拌速率掺入AH-70道路沥青的可行性进行了研究,结果表明在搅拌温度160℃、搅拌时间10 min、搅拌速率2500 r·min-1的条件下,向AH-70道路沥青中掺入1%的重质馏分,可以基本达到AH-70沥青的标准,与此同时其老化后的延展性还能得到很大改善。
以上研究成果,为热解油的资源化利用开辟了一条新的途径,具有重要的学术意义和应用价值。
Large amount of used tires have been produced due to the rapidly growing global economics and automobile industry. To figure out an economic and practical manner on utilization of used tires has come into a stringent task for researches. It is widely known that to pyrolysis used tires is a high value-added and environmentally friendly recycling route. However, the most critical issue during used tires pyrolysis is how to intelligently utilize the specific pyrolysis oil. In this dissertation, used tires pyrolysis oil from industrial unit was used as the starting material. Characterization, utilization and application of used tire pyrolysis oil were studied. The results are expected to provide a principle valuable option for the utilization of used tires. This dissertation mainly consists of the following contents.
A detail analysis and evaluation were conducted on compositions of the used tire pyrolysis oil, including fractions and narrow fractions of the oil. The results showed that pyrolysis oil was low metal content with high sulfur and nitrogen, and high aromatic. The content of light and medium fractions was high up to 62.9% of pyrolysis oil, and the characteristics and compositions were much closed to those of FCC gasoline and FCC (Fluid Catalytic Cracking) diesel, respectively. On the other hand, the characteristics and compositions of heavy fraction were similar to those of petroleum asphalt. The regular pattern of the distribution of hydrocarbon compounds and non-hydrocarbon compounds in narrow fractions were ascertained as well. In the characteristics component analysis of the pyrolysis oil, it was found that the main acidic compounds in the pyrolysis oil were fatty acids which are seldom seen in crude oils.
Pyrolysis oil contained light and medium fractions of 62.9%, which was an important point for utilization of pyrolysis oil. Since the characteristics and compositions of pyrolysis oil were similar to those of crude oil, it is potential to use oil processing methods to process and turn the pyrolysis oil into petroleum products or additive particles. In this dissertation, a distinctive utilization route for the pyrolysis oil was present, which the pyrolysis oil would be incorporated in oil processing plants in consideration of the features of pyrolytic device being small scale and large dispersion.
Light fraction in the pyrolysis oil was used as a model fraction to blend with FCC gasoline, and then the hydrotreating process of the mixture oil was studied. With the method of orthogonal experiment, the hydrotreating operation parameters (including the blending ratio of light fraction to FCC gasoline) on desulphurization and denitrogeneration rate were optimized in the laboratory fixed bed micro-reactor. The results showed that hydrotreating temperature was the most significant factor. Furthermore, the feasibility of hydrotreating of FCC light gasoline blending with light fraction was investigated under industrial operating conditions. The results showed that density, sulfur content and distillation range of the hydrotreating product achieved the standards of gasoline fuels for vehicles under the following conditions:the ratio of hydrogen to oil at 512, the liquid hourly space velocity at 1.65 h-1, reaction temperature at 353℃, reaction pressure at 3 MPa, and blending ratio at 10%. In the three kinetic study models of hydrotreating reaction of FCC gasoline blending with light fraction, the first-order reaction kinetic model was found to describe the HDS and HDN reactions. The analysis of relative error and F statistical analysis showed that the multiple correlation indexes were 0.9248 and 0.9794, and the average relative errors were 4.33% and 0.87%, respectively.
The investigation of heavy fraction composition showed that heavy fraction was potential to produce road asphalt. The feasibility of heavy fraction to produce road asphalt was studied by distillation and blending methods, respectively. The distillation results showed that penetration, softening point, and ductility of straight asphalt of cutting point temperature at 420℃,430℃and 440℃could meet with the major technical index of road asphalt's standards, except for substandard performance after aging. Therefore, heavy fraction producing road asphalt by distillation method was infeasible. On the other hand, under conditions of different mixing temperature, stirring time, stirring speed, and the feasibility of AH-70 road asphalts blending with heavy fraction were discussed. The results showed that the aged ductility of the blending asphalt was greatly enhanced, which can basically match the standard of AH-70 road asphalt. The optimum conditions were mixed at 160℃, stirred at 2500 r-min-1 for 10 min with the blending ratio of 1%.
These results open up a novel route for utilization of used tire pyrolysis oil, and have not only significant academic value but also application value.
引文
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