化工学报 ›› 2020, Vol. 71 ›› Issue (11): 5320-5336.DOI: 10.11949/0438-1157.20200332
收稿日期:
2020-03-30
修回日期:
2020-06-10
出版日期:
2020-11-05
发布日期:
2020-11-05
通讯作者:
王志远
作者简介:
王志远(1983—),男,博士,讲师,基金资助:
Zhiyuan WANG(),Xudong DING,Boyan WANG,Zhihong XING
Received:
2020-03-30
Revised:
2020-06-10
Online:
2020-11-05
Published:
2020-11-05
Contact:
Zhiyuan WANG
摘要:
以石脑油为裂解原料,考察了硫化物和硫/磷化合物的添加方式对热裂解结焦行为的影响。采用Raman光谱、XRD、SEM和XPS等检测手段表征了HP40试样的氧化层和焦炭的形貌与结构。结果表明,原料连续注入硫化物条件下,磷化物的加入使得焦炭结构改变,显示出优异的抗结焦效果。硫化物和硫/磷化合物预处理导致氧化层中Fe含量升高,抑制结焦效果有限。硫/磷预处理与原料连续注入硫/磷化合物联合方式与原料连续注入硫/磷化合物方式的抗结焦效果接近,但前者在初期的抑制效果更明显。所有添加方式都会引起结焦层中无定形焦炭含量升高,焦炭的石墨化程度降低。热裂解焦炭缩合程度较高,硫化物和硫/磷化合物减少了催化结焦的生成,在一定程度上提高了焦层中氢含量。
中图分类号:
王志远,丁旭东,王博研,邢志宏. 硫化物和硫/磷化合物的添加方式对石脑油热裂解结焦影响的研究[J]. 化工学报, 2020, 71(11): 5320-5336.
Zhiyuan WANG,Xudong DING,Boyan WANG,Zhihong XING. Addition methods of sulfur and sulfur/phosphorus-based compounds on coking behavior during thermal cracking of naphtha[J]. CIESC Journal, 2020, 71(11): 5320-5336.
参数 | 数值 |
---|---|
空气预氧化实验 | |
温度/K | 1073 |
空气流量/(ml/min) | 700 |
时间/min | 600 |
清焦 | |
温度/K | 1073-1123 |
空气流量/(ml/min) | 500 |
时间/min | 20 |
硫化物和硫/磷化合物预处理实验 | |
温度/K | 1103 |
去离子水流量/(ml/min) | 1 |
DMDS质量浓度/(μg/gwater) | 500 |
TPPI质量浓度/(μg/gwater) | 100 |
时间/min | 120 |
热裂解实验 | |
温度/K | 1123 |
石脑油流量/(ml/min) | 2 |
去离子水流量/(ml/min) | 0.7 |
表1 实验参数
Table 1 Experimental conditions for each experimental step
参数 | 数值 |
---|---|
空气预氧化实验 | |
温度/K | 1073 |
空气流量/(ml/min) | 700 |
时间/min | 600 |
清焦 | |
温度/K | 1073-1123 |
空气流量/(ml/min) | 500 |
时间/min | 20 |
硫化物和硫/磷化合物预处理实验 | |
温度/K | 1103 |
去离子水流量/(ml/min) | 1 |
DMDS质量浓度/(μg/gwater) | 500 |
TPPI质量浓度/(μg/gwater) | 100 |
时间/min | 120 |
热裂解实验 | |
温度/K | 1123 |
石脑油流量/(ml/min) | 2 |
去离子水流量/(ml/min) | 0.7 |
流程 | 方案 |
---|---|
空气预氧化处理 | preoxidation |
采用DMDS预处理 | Pre S |
采用DMDS& TPPI预处理 | Pre S/P |
原料连续添加 DMDS+ thiophene+benzothiophene+TEP | sulfides/TEP |
原料连续添加 DMDS+thiophene+benzothiophene+TPPI | sulfides/TPPI |
采用DMDS预处理,随后原料连续添加 DMDS | Pre S + S |
采用DMDS& TPPI预处理,随后原料连续添加DMDS+thiophene+benzothiophene+TPPI | Pre S/P + sulfides/TPPI |
表2 实验方案
Table 2 Experimental plans for each experimental step
流程 | 方案 |
---|---|
空气预氧化处理 | preoxidation |
采用DMDS预处理 | Pre S |
采用DMDS& TPPI预处理 | Pre S/P |
原料连续添加 DMDS+ thiophene+benzothiophene+TEP | sulfides/TEP |
原料连续添加 DMDS+thiophene+benzothiophene+TPPI | sulfides/TPPI |
采用DMDS预处理,随后原料连续添加 DMDS | Pre S + S |
采用DMDS& TPPI预处理,随后原料连续添加DMDS+thiophene+benzothiophene+TPPI | Pre S/P + sulfides/TPPI |
加速电压/ kV | 分析区域 | Cr原子浓度/% | Mn原子浓度/% | Fe原子浓度/% | Ni原子浓度/% | O原子浓度/% | Si原子浓度/% |
---|---|---|---|---|---|---|---|
10(h≤0.53 μm) | Ⅰ | 13.66 | 2.25 | 1.83 | — | 82.25 | — |
Ⅱ | 13.76 | 1.85 | 1.50 | — | 82.88 | — | |
Ⅲ | 16.86 | 1.71 | — | — | 81.42 | — | |
15(h≤1.04 μm) | I | 25.36 | 3.47 | 6.97 | 4.42 | 58.35 | 1.40 |
Ⅱ | 27.58 | 3.56 | 4.48 | 2.05 | 61.44 | 0.88 | |
Ⅲ | 31.46 | 3.07 | 2.89 | 1.53 | 59.54 | 1.50 |
表3 不同预处理条件下HP40合金表面氧化层元素分布
Table 3 Element concentrations of the oxide films on HP40 alloys
加速电压/ kV | 分析区域 | Cr原子浓度/% | Mn原子浓度/% | Fe原子浓度/% | Ni原子浓度/% | O原子浓度/% | Si原子浓度/% |
---|---|---|---|---|---|---|---|
10(h≤0.53 μm) | Ⅰ | 13.66 | 2.25 | 1.83 | — | 82.25 | — |
Ⅱ | 13.76 | 1.85 | 1.50 | — | 82.88 | — | |
Ⅲ | 16.86 | 1.71 | — | — | 81.42 | — | |
15(h≤1.04 μm) | I | 25.36 | 3.47 | 6.97 | 4.42 | 58.35 | 1.40 |
Ⅱ | 27.58 | 3.56 | 4.48 | 2.05 | 61.44 | 0.88 | |
Ⅲ | 31.46 | 3.07 | 2.89 | 1.53 | 59.54 | 1.50 |
图5 裂解时间1 h条件下,未添加/添加二甲基二硫后HP40合金氧化层表面碳纤维的SEM图
Fig.5 SEM images of carbon fibers on HP40 alloys in the absence/presence of DMDS after cracking time of 1 h
图7 裂解时间1 h和3 h条件下,添加硫化物后HP40合金表面焦炭沉积量情况
Fig.7 The amounts of coke formed on HP40 alloys with the addition of sulfides after cracking time of 1 h and 3 h
图8 裂解时间1 h和3 h、实验方案为“Pre S/P”条件下,HP40合金表面焦炭的SEM图和丝状焦的EDS分析
Fig.8 SEM images of cokes on HP40 alloys under the condition of “ Pre S/P” after cracking time of 1h and 3 h; EDS of cokes on HP40 alloys
图9 裂解时间1 h和3 h、实验方案为Pre S条件下,HP40合金表面焦炭的SEM图和表面丝状焦的EDS分析
Fig.9 SEM images of cokes on HP40 alloys under the condition of Pre S after cracking time of 1h and 3 h;EDS of cokes on HP40 alloys
图10 裂解时间1 h和3 h条件下,不同添加方式对HP40合金表面焦炭沉积量的影响
Fig.10 The amounts of coke formed on HP40 alloys with varying the addition methods after cracking time of 1 h and 3 h
图11 裂解时间1 h和3 h、实验方案为Pre S + S条件下HP40合金表面焦炭的SEM图和表面丝状焦的EDS分析
Fig.11 SEM images of cokes on HP40 alloys under the condition of Pre S + S after cracking time of 1 h and 3 h; EDS of coke on HP40 alloys
图12 裂解时间1 h和3 h条件下,硫/磷组分预处理与原料连续注入硫/磷化合物联合操作方式下HP40合金表面焦炭的SEM图
Fig.12 SEM photos of cokes on HP40 alloys with the pretreatment of DMDS/TPPI followed by continuous addition of mixed sulfides/TPPI after cracking time of 1 h and 3 h
拟合峰 | Raman位移/cm-1 | 振动模式 | 拟合方式 |
---|---|---|---|
G | 1580 | 理想石墨晶格 (E2g-symmetry) | Lorentzian |
D1 | 1350 | 无序石墨晶格 (graphene layer edge, A1g-symmetry) | Lorentzian |
D2 | 1620 | 无序石墨晶格(surface graphene layers, E2g-symmetry) | Lorentzian |
D3 | 1500 | 无定形碳 | Gaussian |
D4 | 1200 | 无序石墨晶格(A1g-symmetry), polyenes, ionic impurities | Lorentzian |
表4 热裂解结焦一阶拉曼光谱的分峰拟合参数[20-21]
Table 4 The parameters of curve fits for the first-order Raman spectra of cokes on HP40 alloys
拟合峰 | Raman位移/cm-1 | 振动模式 | 拟合方式 |
---|---|---|---|
G | 1580 | 理想石墨晶格 (E2g-symmetry) | Lorentzian |
D1 | 1350 | 无序石墨晶格 (graphene layer edge, A1g-symmetry) | Lorentzian |
D2 | 1620 | 无序石墨晶格(surface graphene layers, E2g-symmetry) | Lorentzian |
D3 | 1500 | 无定形碳 | Gaussian |
D4 | 1200 | 无序石墨晶格(A1g-symmetry), polyenes, ionic impurities | Lorentzian |
样品 | ΓD1 /cm-1 | ΓD2 /cm-1 | ΓD3 /cm-1 | ΓD4/cm-1 | ΓG/cm-1 | ID1/IG | ID3/IG | IG/IAll |
---|---|---|---|---|---|---|---|---|
preoxidation | 167.02 | 23.32 | 171.24 | 112.63 | 58.04 | 2.54 | 0.47 | 0.27 |
DMDS | 179.87 | 32.68 | 160.33 | 110.39 | 59.51 | 3.05 | 0.50 | 0.23 |
thiophene | 157.91 | 39.13 | 173.89 | 106.49 | 56.41 | 3.51 | 0.68 | 0.18 |
benzothiophene | 182.63 | 37.72 | 150.61 | 120.18 | 63.15 | 3.59 | 0.52 | 0.21 |
sulfides/TPPI | 178.29 | 35.27 | 163.70 | 114.37 | 58.09 | 3.76 | 0.78 | 0.12 |
Pre S | 150.36 | 38.29 | 170.56 | 126.80 | 57.73 | 2.84 | 0.58 | 0.23 |
Pre S+ sulfides | 173.09 | 39.38 | 157.12 | 124.15 | 62.63 | 3.61 | 0.56 | 0.18 |
Pre S/P | 163.53 | 34.37 | 169.85 | 116.62 | 58.74 | 2.70 | 0.47 | 0.25 |
Pre S/P+sulfides/TPPI | 156.61 | 42.41 | 180.63 | 138.05 | 56.54 | 4.14 | 0.90 | 0.08 |
表5 热裂解结焦拉曼光谱的分峰拟合结果
Table 5 Fitting results of Raman spectra of coke deposits
样品 | ΓD1 /cm-1 | ΓD2 /cm-1 | ΓD3 /cm-1 | ΓD4/cm-1 | ΓG/cm-1 | ID1/IG | ID3/IG | IG/IAll |
---|---|---|---|---|---|---|---|---|
preoxidation | 167.02 | 23.32 | 171.24 | 112.63 | 58.04 | 2.54 | 0.47 | 0.27 |
DMDS | 179.87 | 32.68 | 160.33 | 110.39 | 59.51 | 3.05 | 0.50 | 0.23 |
thiophene | 157.91 | 39.13 | 173.89 | 106.49 | 56.41 | 3.51 | 0.68 | 0.18 |
benzothiophene | 182.63 | 37.72 | 150.61 | 120.18 | 63.15 | 3.59 | 0.52 | 0.21 |
sulfides/TPPI | 178.29 | 35.27 | 163.70 | 114.37 | 58.09 | 3.76 | 0.78 | 0.12 |
Pre S | 150.36 | 38.29 | 170.56 | 126.80 | 57.73 | 2.84 | 0.58 | 0.23 |
Pre S+ sulfides | 173.09 | 39.38 | 157.12 | 124.15 | 62.63 | 3.61 | 0.56 | 0.18 |
Pre S/P | 163.53 | 34.37 | 169.85 | 116.62 | 58.74 | 2.70 | 0.47 | 0.25 |
Pre S/P+sulfides/TPPI | 156.61 | 42.41 | 180.63 | 138.05 | 56.54 | 4.14 | 0.90 | 0.08 |
方案 | sp3/sp2比值 |
---|---|
preoxidation | 0.17 |
sulfides/TPPI | 0.23 |
DMDS | 0.29 |
表6 热裂解结焦的sp3/sp2比值
Table 6 sp3/sp2ratio of coke deposits
方案 | sp3/sp2比值 |
---|---|
preoxidation | 0.17 |
sulfides/TPPI | 0.23 |
DMDS | 0.29 |
方案 | H/C 比值 |
---|---|
preoxidation | 0.69 |
sulfides/TPPI | 2.56 |
连续添加DMDS | 1.25 |
Pre S | 0.82 |
表7 热裂解结焦的H/C比值(质量比)
Table 7 TheH/C massratios of coke deposits
方案 | H/C 比值 |
---|---|
preoxidation | 0.69 |
sulfides/TPPI | 2.56 |
连续添加DMDS | 1.25 |
Pre S | 0.82 |
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