论文总字数:8555字
摘 要
本文采用气相色谱-质谱分析技术研究了93#汽油经H2O2–H3PW12O40–HCl脱硫剂氧化后的93#汽油成分。实验结果表明,经过H2O2-HCl-H3O40PW12·xH2O脱硫剂脱硫后的汽油成分未发生明显改变。关键词:气相色谱-质谱,93#汽油,H2O2,H3O40PW12·xH2O,成分
Abstract:The compositions of gasoline 93# and gasoline 93# oxidized by H2O2-HCl-H3O40PW12 xH2O were studied using gas chromatography - mass spectrometry technology in this paper. The results showed that compositions of gasoline 93# oxidized by H2O2-HCl-H3O40PW12 xH2O did not change obviously.
Keywords: Gas chromatography-mass spectrometry, gasoline 93#, H2O2,H3O40PW12·xH2O, composition
目 录
1 前言 3
2 实验部分 3
2.1 仪器与试剂 3
2.2 仪器分析条件 3
2.3 实验方法 3
3 结果与讨论 4
3.1 色谱图 4
3.2 93#汽油成分分析 4
3.3 氧化处理后的汽油成分分析 9
结 论 15
参 考 文 献 16
致 谢 17
1 前言
燃料油中的含硫化合物是环境污染的主要来源,燃烧后生成的SOx排放到大气中形成酸雨,酸雨是困扰全球的环境问题之一,对环境和人体健康造成很大的伤害。目前,目前存在的脱硫方法主要有催化加氢脱硫[1,2]、氧化脱硫[3-5]、吸附脱硫[6]、生物催化脱硫[7]、萃取脱硫[8]等诸多方法。传统脱硫法是指加氢脱硫法,与传统脱硫方法相比,氧化脱硫具有操作条件温和,成本低等优点,成为近年来发展最快的非加氢脱硫技术。氧化脱硫(ODS)是近年来发展起来的生产超低硫燃料的新技术,可在常温常压下进行,不耗费氢气,设备投资较少,对催化加氢难以脱除的苯并噻吩类化合物有较高的脱硫效率,是一项非常有前途的脱硫技术。
本文以H2O2-HCl脱硫剂氧化汽油,采用气相色谱-质谱方法研究了汽油的成分变化。
2 实验部分
2.1 仪器与试剂
37%HCl;30% H2O2;N,N-二甲基甲酰胺,试剂均为分析纯。
恒温水浴锅;磁力搅拌器; GC—MS一2010 Ultra气质联用仪(岛津公司)。
2.2 仪器分析条件
色谱柱是Rtx-1ms弹性石英毛细管柱 ,柱长30.0m 内径0.25mm 膜厚0.25μm。 色谱柱温40℃开始保持8分钟, 12℃每分钟升到300℃保持5分钟, 进样口温度300℃, 分流进样比50比1 ,进样量0.2μL, 柱流量每分钟0.88ml 。
质谱离子源温度200℃, 接口温度200℃, 溶剂切出时间3分钟, 检测器电压1000v ,扫描范围30到1000。
2.3 实验方法
将10% H2O210.00ml,10.00ml37%HCl,93#汽油10.00ml加入圆底烧瓶中,置于恒温水浴中,保持35℃的反应温度,在磁力搅拌的作用下反应4.00h,反应结束后,取出反应物在室温下静置,分出油相,用10ml水洗三次,10.00ml N,N-二甲基甲酰胺洗三次,取上清液1.00ml用三氯甲烷定容至10.00ml,从中取0.20l按2.2仪器分析条件,用气质联用仪和气相色谱仪定性分析。
3 结果与讨论
3.1 色谱图
93#汽油样品经氧化处理前后的色谱图见图1和图2,可以看出,汽油处理前后其主要成分未发生明显改变。
图1 93#汽油原油谱图
图2 93#汽油相谱图
3.2 93#汽油成分分析
未经过氧化处理的汽油经过质谱检索得到的主要成分见下表1,从表1中我们可以发现,共检出74种有机物质,其中烷烃15种,烯和炔烃共20种,其它的有机物有39种,其主要成分为C2-C19烃类物质。
表1 93#汽油的主要成分分析
No. 相似度 | 保留时间(min) | 分子式 | 分子结构 |
1 89 | 3.050 | C7H16 | |
2 93 | 3.145 | C7H14 | |
3 95 | 3.270 | C7H14 | |
4 89 | 3.390 | C13H26 | |
5 97 | 3.480 | C8H16 | |
6 93 | 3.565 | C7H16 | |
7 89 | 3.595 | C7H12 | |
8 95 | 3.645 | C7H8 | |
9 89 | 3.710 | C10H20 | |
10 94 | 3.775 | C8H18 | |
11 92 | 3.865 | C8H8 | |
12 96 | 3.905 | C8H16 | |
13 97 | 4.030 | C8H16 |
|
14 95 | 4.060 | C8H16 | |
15 87 | 4.110 | C8H14 | |
16 93 | 4.145 | C8H16 | |
17 93 | 4.180 | C8H18 | |
18 96 | 4.225 | C8H16 | |
19 91 | 4.270 | C8H14 | |
20 88 | 4.320 | C9H18 | |
21 89 | 4.440 | C8H16 | |
22 87 | 4.485 | C19H20 | |
23 94 | 4.520 | C8H16 | |
24 91 | 4.565 | C12H26O | |
25 83 | 4.615 | C10H18O | |
26 91 | 4.650 | C9H20 | |
27 90 | 4.730 | C9H18 | |
28 89 | 4.805 | C8H10 | |
29 95 | 4.845 | C9H18 | |
30 96 | 4.915 | C8H10 | |
31 91 | 5.010 | C12H24 | |
32 95 | 5.105 | C9H20 | |
33 92 | 5.160 | C9H18 | |
34 94 | 5.205 | C8H10 | |
35 90 | 5.290 | C9H18 | |
36 93 | 5.375 | C9H18 | |
37 92 | 5.460 | C11H24 | |
38 94 | 5.540 | C9H18 | |
39 78 | 5.635 | C28H30N2 | |
40 88 | 5.700 | C29H40O | |
41 92 | 5.795 | C9H20 | |
42 92 | 5.915 | C10H22 | |
43 81 | 6.005 | C15H13FO | |
44 96 | 6.095 | C9H12 | |
45 94 | 6.195 | C9H12 | |
46 91 | 6.255 | C12H26O | |
47 93 | 6.290 | C10H22 | |
48 88 | 6.320 | C9H12 | |
49 93 | 6.375 | C10H22 | |
50 96 | 6.510 | C9H12 | |
51 88 | 6.565 | C13H14 | |
52 92 | 6.725 | C12H26O | |
53 94 | 6.855 | C9H12 | |
54 87 | 6.995 | C9H10 | |
55 90 | 7.090 | C14H30 | |
56 85 | 7.220 | C10H14 | |
57 93 | 7.300 | C10H14 | |
58 85 | 7.430 | C11H24 | |
59 91 | 7.470 | C10H22 | |
60 88 | 7.530 | C10H14 |
|
61 88 | 7.625 | C10H14 | |
62 85 | 7.865 | C10H14 | |
63 92 | 7.925 | C12H26O |
|
64 92 | 8.010 | C10H14 | |
65 94 | 8.050 | C10H14 | |
66 89 | 8.140 | C12H26O | |
67 88 | 8.250 | C10H12 | |
68 91 | 8.365 | C10H12 | |
69 81 | 8.410 | C10H14 |
|
70 77 | 8.510 | C11H16 | |
71 73 | 8.660 | C19H39Cl | |
72 88 | 8.810 | C11H14 | |
73 80 | 8.920 | C11H14 | |
74 82 | 9.045 | C20H41Cl |
3.3 氧化处理后的汽油成分分析
经过氧化处理后的93#汽油经过仪器质谱检索出的主要成分见表2,可以从表2中得出,共被检测出91种物质,其中烷烃13种,烯烃和炔烃共有25种,其它有机物共有53种,其主要成分为C2-C19烃类物质。
No. | 相似度 | 保留时间(min) | 分子式 | 分子结构 |
1 | 89 | 3.050 | C7H16 | |
2 | 88 | 3.150 | C7H14 | |
3 | 96 | 3.270 | C7H14 | |
4 | 89 | 3.290 | C13H26 | |
5 | 97 | 3.485 | C8H16 | |
6 | 91 | 3.565 | C8H16 | |
7 | 89 | 3.600 | C7H12 | |
8 | 94 | 3.645 | C7H18 | |
9 | 89 | 3.715 | C10H20 | |
10 | 93 | 3.775 | C8H18 | |
11 | 92 | 3.865 | C8H18 | |
12 | 96 | 3.910 | C8H16 | |
13 | 90 | 4.005 | C8H16 | |
14 | 97 | 4.035 | C8H16 | |
15 | 96 | 4.060 | C8H16 | |
16 | 87 | 4.115 | C8H14 | |
17 | 93 | 4.150 | C8H16 | |
18 | 93 | 4.185 | C8H18 | |
19 | 96 | 4.230 | C8H16 | |
20 | 91 | 4.275 | C8H14 | |
21 | 88 | 4.320 | C11H22 | |
22 | 80 | 4.395 | C10H18O | |
23 | 88 | 4.445 | C8H16 | |
24 | 87 | 4.485 | C9H20 | |
25 | 93 | 4.525 | C8H16 | |
26 | 91 | 4.570 | C17H29F5 | |
27 | 82 | 4.620 | C11H20 | |
28 | 92 | 4.655 | C12H24 | |
29 | 90 | 4.735 | C9H18 | |
30 | 88 | 4.810 | C8H10 | |
31 | 94 | 4.845 | C9H18 | |
32 | 95 | 4.915 | C8H10 | |
33 | 83 | 4.975 | C9H18O | |
34 | 91 | 5.015 | C9H20 | |
35 | 91 | 5.165 | C9H18 | |
36 | 93 | 5.205 | C8H10 | |
37 | 90 | 5.290 | C9H18 | |
38 | 93 | 5.380 | C9H18 | |
39 | 91 | 5.460 | C11H24 | |
40 | 89 | 5.505 | C9H18 | |
41 | 93 | 5.545 | C9H18 | |
42 | 78 | 5.640 | C14H16O2 | |
43 | 88 | 5.705 | C19H40O | |
44 | 91 | 5.800 | C19H40 | |
45 | 91 | 5.850 | C20H40O | |
46 | 92 | 5.915 | C10H22 | |
47 | 79 | 6.010 | C14H20O3 | |
48 | 96 | 6.100 | C9H12 | |
49 | 92 | 6.195 | C9H12 | |
50 | 91 | 6.260 | C12H26O | |
51 | 93 | 6.290 | C10H22 | |
52 | 87 | 6.325 | C9H12 | |
53 | 93 | 6.375 | C10H22 | |
54 | 96 | 6.515 | C9H12 | |
55 | 85 | 6.565 | C10H20 | |
56 | 87 | 6.620 | C9H18 | |
57 | 91 | 6.725 | C12H26O | |
58 | 94 | 6.855 | C9H12 | |
59 | 89 | 6.920 | C14H30O | |
60 | 88 | 7.000 | C9H10 | |
61 | 91 | 7.090 | C15H32 | |
62 | 88 | 7.165 | C14H30O | |
63 | 86 | 7.225 | C10H14 | |
64 | 93 | 7.300 | C10H14 | |
65 | 81 | 7.430 | C12H26O | |
66 | 90 | 7.470 | C11H24 | |
67 | 89 | 7.535 | C10H14 | |
68 | 88 | 7.590 | C11H24 | |
69 | 87 | 7.630 | C10H14 |
|
70 | 75 | 7.710 | C10H18O2 | |
71 | 88 | 7.805 | C17H33Cl | |
72 | 84 | 7.870 | C10H14 | |
73 | 91 | 7.925 | C12H25I | |
74 | 91 | 8.010 | C10H14 | |
75 | 93 | 8.050 | C10H14 | |
76 | 88 | 8.140 | C12H26O | |
77 | 87 | 8.255 | C10H12 | |
78 | 73 | 8.330 | C26H46 | |
79 | 91 | 8.370 | C10H12 | |
80 | 81 | 8.415 | C10H14 | |
81 | 72 | 8.515 | C11H16 | |
82 | 72 | 8.565 | C20H41Cl | |
83 | 71 | 8.660 | C19H39Cl | |
84 | 75 | 8.730 | C22H33Cl | |
85 | 86 | 8.810 | C11H14 | |
86 | 75 | 8.925 | C11H14 | |
87 | 91 | 10.480 | C12H36O6 | |
88 | 78 | 12.010 | C10H22O | |
89 | 86 | 12.160 | C14H42O7 | |
90 | 75 | 13.635 | C16H50O7 | |
91 | 75 | 13.715 | C10H22O |
结 论
经过对汽油及经氧化处理后的汽油进行色谱-质谱分析研究表明,得出原油中共74种有机化合物,而经过氧化反应后的柴油中共检测出91种有机化合物,在氧化前后的主要成分未见到明显变化。汽油经脱硫剂氧化后含氯的有机物未被检出,表明氯离子没有参与此反应。
参 考 文 献
[1] 达建文,韩新竹,徐兴忠等. 催化裂化柴油选择性加氢脱硫催化剂的研制及性能评价[J].石油炼制
与化工.2002,33(7):1-4.
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