城市污泥热解液相产物分析及焦油加氢精制
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摘要
文章以乙酸钾为催化剂,利用间歇式反应釜热解制备城市污泥的液相产物。采用CH_2Cl_2萃取分离液相产物中的油相(焦油)和水相,并进一步对焦油加氢精制获取轻质油。结果表明:污泥单独热解时水相产物呈碱性,密度接近于水,低温90～300℃时焦油含量极少;温度增至400～500℃时,焦油和水相氨氮含量分别高达8.18%和7 990.80 mg/L。在污泥中添加不同种类生物质(花生壳、玉米秆、玉米芯、稻草)共热解后,焦油含量均显著增加,水相(木醋液)均呈酸性,其氨氮含量均下降。与污泥-花生壳共热解制备的焦油相比,加氢精制的轻质油为密度和运动粘度显著降低的浅黄色液体,胶质和沥青质含量明显减小,汽、柴馏分总收率高达86.1%,硫氮含量降低,净热值增大。通过色谱质谱联用仪测定木醋液,其有机物主要包含酚类、酮类。
The liquid phase products were produced from pyrolysis of municipal sludge using a batch reactor with the potassium acetate as catalyst. The oil phase(tar) and aqueous phase were extracted from the liquid phase products using CH_2Cl_2 solvent as extractant, and then the hydrofining process of tar was conducted to obtain light oil. The results showed that when the sludge was individually pyrolyzed at the low temperature of 90～300 ℃, alkaline aqueous phase product with the density close to water was obtained, along with few tar. When the pyrolysis temperature was increased to 400～500 ℃, the contents of tar and ammonia-nitrogen in the aqueous phase reached up to 8.18% and 7 990.80 mg/L, respectively. After adding different kinds of biomass(peanut shell, corn stalk, corn cob and straw), the aqueous phase(wood vinegar liquid) was acidic, and the tar content significantly increased, but the ammonia & nitrogen content decreased. Compared with the tar produced by co-pyrolysis of sludge and peanut shell, a light yellow liquid from the hydrorefining of tar was obtained, with the density and kinematic viscosity significantly reducing. Four components analysis experiments revealed that the resin & asphaltene decreased obviously and the total yield of gasoline & diesel fractions reached up to 86.1%.Furthermore, the content of sulfur & nitrogen decreased, and the net calorific value increased. The organics vinegar liquid was determined by chromatograph-mass spectrometer, which mainly included phenols and ketones.
The liquid phase products were produced from pyrolysis of municipal sludge using a batch reactor with the potassium acetate as catalyst. The oil phase(tar) and aqueous phase were extracted from the liquid phase products using CH_2Cl_2 solvent as extractant, and then the hydrofining process of tar was conducted to obtain light oil. The results showed that when the sludge was individually pyrolyzed at the low temperature of 90～300 ℃, alkaline aqueous phase product with the density close to water was obtained, along with few tar. When the pyrolysis temperature was increased to 400～500 ℃, the contents of tar and ammonia-nitrogen in the aqueous phase reached up to 8.18% and 7 990.80 mg/L, respectively. After adding different kinds of biomass(peanut shell, corn stalk, corn cob and straw), the aqueous phase(wood vinegar liquid) was acidic, and the tar content significantly increased, but the ammonia & nitrogen content decreased. Compared with the tar produced by co-pyrolysis of sludge and peanut shell, a light yellow liquid from the hydrorefining of tar was obtained, with the density and kinematic viscosity significantly reducing. Four components analysis experiments revealed that the resin & asphaltene decreased obviously and the total yield of gasoline & diesel fractions reached up to 86.1%.Furthermore, the content of sulfur & nitrogen decreased, and the net calorific value increased. The organics vinegar liquid was determined by chromatograph-mass spectrometer, which mainly included phenols and ketones.
引文
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[3]何品晶,顾国维,李笃中.城市污泥处理与利用[M].北京:科学出版社,2003.300-308.
[4]李刚,王格格,王忠科,等.脱水污泥低温热解制备生物炭的研究[J].可再生能源,2016,34(10):1533-1539.
[5]Méndez A,Paz-Ferreiro J,Araujo F,et al.Biochar from pyrolysis of deinking paper sludge and its use in the treatment of a nickel polluted soil[J].Journal of Analytical&Applied Pyrolysis,2014,107(5):46-52.
[6]Devi P,Saroha A K.Risk analysis of pyrolyzed biochar made from paper mill effluent treatment plant sludge for bioavailability and eco-toxicity of heavy metals[J].Bioresource Technology,2014,162(162C):308-315.
[7]郭秀兰,黄鹤,周强,等.生物质焦油裂解催化剂研究进展[J].可再生能源,2004(1):9-13.
[8]任善普,宋强,张蒙蒙,等.城市生活垃圾热解焦对热解焦油的影响[J].可再生能源,2016,34(8):1233-1238.
[9]施庆燕,李兵,赵由才.污泥低温热解制油的影响因素[J].环境卫生工程,2006,14(5):4-6.
[10]王忠科,陆江银,王建俊.响应面法优化污泥-花生壳共热解工艺条件[J].环境工程学报,2017,1(10):5663-5670.
[11]Zhang D,Duan A,Zhao Z,et al.Synthesis,characterization,and catalytic performance of Ni Mo catalysts supported on hierarchically porous Beta-KIT-6 material in the hydrodesulfurization of dibenzothiophene[J].Journal of Catalysis,2010,274(2):273-286.
[12]Meng J,Wang Z,Ma Y,et al.Hydrocracking of lowtemperature coal tar over NiMo/Beta-KIT-6 catalyst to produce gasoline oil[J].Fuel Processing Technology,2017,165:62-71.
[13]金湓,李宝霞.生物质与污水污泥共热解特性研究[J].可再生能源,2014,32(2):234-239.
[14]尹龙晓,周兴求,伍健东,等.污泥与秸秆掺烧的燃烧特性研究及应用[J].可再生能源,2013,31(1):71-75.
[15]A Ba觭aoui,A Yaacoubi,A Dahbi,et al.Optimization of conditions for the preparation of activated carbons from olive-waste cakes[J].Carbon,2001,39(3):425-432.
[16]陈曼.城市污水污泥热解特性与转化机理的研究[D].南京:东南大学,2006.
[17]何文君.不同木醋液生物活性的比较研究[D].杨凌:西北农林科技大学,2010.
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