离子液体/H<sub>2</sub>O<sub>2</sub>体系脱硫实验研究

李梅; 孙功成; 程雪云; 李佳佳; 金权; 徐荣声

离子液体/H₂O₂体系脱硫实验研究

李梅^{1, 2, 3, ,},
孙功成¹,
程雪云¹,
李佳佳¹,
金权¹,
徐荣声¹

1.
北方民族大学化学与化学工程学院, 宁夏银川 750021
2.
北方民族大学宁夏太阳能化学转化技术重点实验室, 宁夏银川 750021
3.
北方民族大学国家民委化工技术基础重点实验室, 宁夏银川 750021

基金项目:

国家自然科学基金 21666001

北方民族大学校级科研项目 2017HG04

北方民族大学校级重大专项 ZDZX201803

北方民族大学科研平台项目 201707

详细信息

中图分类号: TQ530.2
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- 被引次数: 0
出版历程
- 收稿日期: 2019-05-20
- 修回日期: 2019-07-08
- 网络出版日期: 2021-01-23
- 刊出日期: 2019-09-10

Experimental study on desulfurization by ionic liquids/H₂O₂ system

1.
School of Chemistry and Chemical Engineering, North Minzu University, Yinchuan 750021, China
2.
Ningxia Key Laboratory of Solar Chemical Conversion Technology, North Minzu University, Yinchuan 750021, China
3.
Key Laboratory for Chemical Engineering and Technology, State Ethnic Affairs Commission, North Minzu University, Yinchuan 750021, China

Funds:

the National Natural Science Foundation of China 21666001

North Minzu University-Level Scientific Research Project 2017HG04

North Minzu University-Level Major Project ZDZX201803

North Minzu University Research Platform Project 201707

More Information

Corresponding author: LI Mei, Tel: 15009663719, E-mail: echolimei@126.com

摘要

摘要: 选取四种不同种类离子液体（ILs），1-丁基-3-甲基咪唑溴化物（[Bmim]Br）、1-丁基-3-甲基咪唑四氟硼酸盐（[Bmim]BF₄）、1-丁基-3-甲基咪唑硫酸氢盐（[Bmim]HSO₄）、1-丁基-3-甲基咪唑磷酸二氢盐（[Bmim]H₂PO₄）与30% H₂O₂溶液在温和条件下对两种高硫脱灰煤样（LS、QX）进行脱硫实验研究。用化学法测定脱硫前后煤样形态硫含量，并利用傅里叶变换红外光谱（FT-IR）、X射线光电子能谱（XPS）、扫描电子显微镜（SEM）及热重（TG）对脱硫前后的煤样进行表征。结果表明，离子液体的加入使H₂O₂氧化脱硫能力增强，煤中硫铁矿硫和有机硫化物硫被显著脱除；经ILs/H₂O₂体系作用后的煤样中小粒径的颗粒减少，颗粒间的缝隙增大，煤表面的凹坑明显，热重实验结果表明，ILs/H₂O₂体系作用后的煤样相对于原煤热失重增大，部分挥发性物质释放峰温提前。
- 离子液体 /
- 脱硫 /
- 形态硫 /
- 热解特性
Abstract: Four different kinds of ionic liquids(ILs), namely, 1-butyl-3-methylimidazolium bromide([Bmim]Br), 1-butyl-3-methylimidazolium tetrafluoroborate([Bmim]BF₄), 1-butyl-3-methylimidazolium hydro-sulfate([Bmim]HSO₄), and 1-butyl-3-methylimidazolium dihydrophosphate([Bmim]H₂PO₄) were selected to add to the H₂O₂ solution (30%), respectively, to obtain four mixed solutions. Then, two kinds of deashed high-sulfur coal (LS, QX) desulfurization experiments were tested with above mixed solutions under mild conditions, respectively. The contents of different sulfur forms in coal samples before and after desulfurization were determined by wet chemical method, and the coal samples before and after desulfurization were characterized using Fourier transform infrared spectroscopy (FT-IR), X-ray photoelectron spectroscopy (XPS), scanning electron microscope (SEM), and thermogravimetric (TG). The results show that the addition of ionic liquids can make the H₂O₂ oxidation desulfurization ability enhance, and pyrite sulfur and organic sulfide sulfur in coal are obviously removed. After treated by the ILs/H₂O₂ system, the small size particle decreases, the space among the particles increases, and the pits on the coal surface become obvious. Moreover, the thermogravimetric test results show that the total weight loss of the coal sample treated by the ILs/H₂O₂ system increases and the peak temperature of some volatile substances lowers.
- ionic liquids /
- desulfurization /
- sulfur forms /
- pyrolysis characteristics

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图 1 离子液体结构图

Figure 1 Structure diagram of ionic liquids

(a): [Bmim]Br; (b): [Bmim]BF₄; (c): [Bmim]HSO₄; (d): [Bmim]H₂PO₄

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图 2 H₂O₂及ILs/H₂O₂体系处理LS煤的脱硫率变化

Figure 2 Desulfurization rates of LS coal treated by ILs/H₂O₂ system and H₂O₂

0^#: LS-H₂O₂; 1^#: LS-H₂O₂-[Bmim]Br; 2^#: LS-H₂O₂-[Bmim]BF₄; 3^#: LS- H₂O₂-[Bmim]HSO₄; 4^#: LS-H₂O₂-[Bmim] H₂PO₄

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图 3 H₂O₂及ILs/H₂O₂体系处理QX煤的脱硫率变化

Figure 3 Desulfurization rates of QX coal treated by ILs/H₂O₂ system and H₂O₂

a^#: QX-H₂O₂; b^#: QX-H₂O₂-[Bmim]Br; c^#: QX-H₂O₂-[Bmim]BF₄; d^#: QX- H₂O₂-[Bmim]HSO₄; e^#: QX-H₂O₂-[Bmim] H₂PO₄

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图 4 H₂O₂和ILs/H₂O₂体系脱硫前后煤样的FT-IR谱图

Figure 4 FT-IR spectra of coal samples before and after desulfurized by ILs/H₂O₂ system and H₂O₂

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图 5 H₂O₂和ILs/H₂O₂体系脱硫前后煤样400-700cm^-1的FT-IR谱图

Figure 5 400-700cm^-1 FT-IR spectra of coal samples before and after desulfurized by ILs/H₂O₂ system and H₂O₂

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图 6 H₂O₂和ILs/H₂O₂体系脱硫前后LS煤中硫的XPS谱图

Figure 6 XPS spectra of sulfur in LS coal before and after desulfurized by ILs/H₂O₂ system and H₂O₂

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图 7 H₂O₂和ILs/H₂O₂体系脱硫前后QX煤中硫的XPS谱图

Figure 7 XPS spectra of sulfur in QX coal before and after desulfurized by ILs/H₂O₂ system and H₂O₂

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图 8 H₂O₂和ILs/H₂O₂体系脱硫前后QX煤的SEM照片

Figure 8 SEM spectra of QX coal samples before and after H₂O₂ and ILs/H₂O₂ desulfurization

(a)、(b)、(c)、(d)、(g): QX-Raw, (e)、(h): QX-H₂O₂, (f)、(i): QX-H₂O₂-[Bmim]H₂PO₄

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图 9 ILs/H₂O₂体系脱硫前后煤样的TG-DTG曲线

Figure 9 TG/DTG curves of coal samples before and after desulfurized by ILs/H₂O₂ system and H₂O₂

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表 1 煤样的工业分析和元素分析

Table 1 Proximate and ultimate analyses of coal samples

Sample	Approximate analysis w_ad/%				Ultimate analysis w_ad/%
Sample	M	A	V	FC	C	H	O^*	N	S
LS-raw	0.92	57.00	13.05	29.03	25.28	0.96	10.96	0.69	4.19
QX-raw	2.11	53.60	8.40	35.89	34.95	1.62	1.25	0.62	5.85
note: ad: air dried; M: moisture; A: ash content; V: volatile; FC: fixed carbon; ^*: by difference

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表 2 H₂O₂及ILs/H₂O₂体系作用前后煤样的工业分析和元素分析

Table 2 Proximate and ultimate analyses of deashed coals with and without desulfurization by ILs/H₂O₂ system and H₂O₂

Sample	Approximate analysis w_ad/%				Ultimate analysis w_ad/%
Sample	M	A	V	FC	C	H	O^*	N	S
LS	1.76	5.77	19.48	72.99	76.30	3.26	3.21	1.02	8.68
LS-H₂O₂	3.72	3.35	22.34	70.59	70.75	3.95	11.80	0.85	5.58
LS-H₂O₂-[Bmim]Br	2.28	1.15	23.98	72.59	78.34	3.66	8.95	1.18	4.44
LS-H₂O₂-[Bmim]BF₄	3.86	1.88	24.53	69.73	69.45	4.14	15.80	1.26	3.61
LS- H₂O₂-[Bmim]HSO₄	3.09	2.23	25.11	69.57	70.42	3.44	14.33	1.12	5.37
LS-H₂O₂-[Bmim]H₂PO₄	3.10	1.66	24.81	70.43	72.61	3.84	14.76	1.21	2.82
QX	4.69	11.27	14.78	69.26	58.88	2.43	10.08	0.77	11.88
QX -H₂O₂	3.33	6.62	15.19	74.86	58.94	2.45	20.65	0.78	7.23
QX -H₂O₂-[Bmim]Br	2.80	5.11	17.23	74.86	80.19	2.56	1.51	1.30	6.53
QX -H₂O₂-[Bmim]BF₄	2.91	5.38	17.74	73.97	76.36	2.98	6.01	1.44	4.92
QX - H₂O₂-[Bmim]HSO₄	4.06	4.77	16.93	74.24	71.96	2.21	9.38	1.17	6.45
QX -H₂O₂-[Bmim]H₂PO₄	3.98	4.22	17.79	74.01	70.02	2.40	16.19	1.14	2.05
note: ad: air dried; M: moisture; A: ash content; V: volatile; FC: fixed carbon; ^*: by difference

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表 3 H₂O₂及ILs/H₂O₂体系脱硫前后煤样形态硫的变化

Table 3 Changes of sulfur forms in deashed coals with and without desulfurization by ILs/H₂O₂ system and H₂O₂

Sample	w/%	Sulfur forms w_d/%			Sulfur forms removal η/%
Sample	w/%	S_t	S_p	S_o	η_st	η_sp	η_so
LS	-	8.68	3.82	4.86	-	-	-
LS-H₂O₂	86.28	5.58	2.16	3.42	44.53	43.45	29.63
LS-H₂O₂-[Bmim]Br	94.91	4.44	1.83	2.61	51.45	52.09	46.29
LS-H₂O₂-[Bmim]BF₄	91.00	3.61	1.24	2.37	62.15	67.54	51.23
LS-H₂O₂-[Bmim]HSO₄	70.56	5.37	1.21	4.16	56.66	68.32	14.40
LS-H₂O₂-[Bmim]H₂PO₄	93.64	2.82	0.81	2.01	69.58	78.79	58.64
QX	-	11.88	6.07	5.81	-	-	-
QX-H₂O₂	87.22	7.23	3.32	3.91	46.92	45.30	32.70
QX-H₂O₂-[Bmim]Br	91.02	6.53	3.11	3.42	49.97	48.76	41.13
QX-H₂O₂-[Bmim]BF₄	83.81	4.92	2.01	2.91	65.29	66.89	49.07
QX-H₂O₂-[Bmim]HSO₄	83.29	6.45	2.69	3.76	54.78	55.68	35.28
QX-H₂O₂-[Bmim]H₂PO₄	92.20	2.05	0.22	1.83	84.09	96.37	68.50
note: S_t: total sulfur; S_p: pyrite sulfur; S_o: organic sulfur

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表 4 离子液体单独作用下煤样收率及全硫脱硫率

Table 4 Yield and ratio of total desulfurization of coals after treatment by individual effect of ILs

Sample	w/%	S_t/%	η_St/%
LS	-	8.68	-
LS-H₂O-[Bmim]Br	97.45	8.19	8.05
LS-H₂O-[Bmim]BF₄	97.90	7.99	9.88
LS-H₂O-[Bmim]HSO₄	98.29	8.28	6.24
LS-H₂O-[Bmim]H₂PO₄	97.58	8.17	8.15
QX	-	11.88	-
QX-H₂O-[Bmim]Br	98.35	11.23	7.03
QX-H₂O-[Bmim]BF₄	97.94	11.15	7.42
QX-H₂O-[Bmim]HSO₄	97.76	10.97	9.73
QX-H₂O-[Bmim]H₂PO₄	95.31	10.62	14.80

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表 5 XPS谱图中LS样品的硫形态及相对含量

Table 5 Sulfur form and its relative content in LS samples by XPS spectra

	Binding energy E/eV	Sulfur form	a/%	b/%	c/%	d/%	e/%	f/%
Peak 1	163.6-164.0	pyrite	28.78	19.33	14.43	10.76	9.79	5.94
Peak 2	164.0-164.4	thiophene	31.33	26.72	37.39	31.68	25.34	27.34
Peak 3	165.0-166.0	sulfoxide	30.89	26.93	27.66	30.55	28.82	30.31
Peak 4	167.5-168.5	sulfone	9.00	27.02	20.52	27.01	36.05	36.41
a: LS; b: LS-H₂O₂; c: LS-H₂O₂-[Bmim]Br; d: LS-H₂O₂-[Bmim]BF₄; e: LS-H₂O₂-[Bmim]HSO₄; f: LS-H₂O₂-[Bmim]H₂PO₄

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表 6 XPS谱图中QX样品的硫形态及相对含量

Table 6 Sulfur form and its relative content in QX samples by XPS spectra

	Binding energy E/eV	Sulfur form	a/%	b/%	c/%	d/%	e/%	f/%
Peak 1	162.2-163.2	organic sulfide	11.90	8.69	10.78	6.68	5.77	-
Peak 2	163.6-164.0	pyrite	20.28	13.00	12.59	11.81	8.87	12.11
Peak 3	164.0-164.4	thiophene	24.70	17.88	19.25	21.70	18.73	36.33
Peak 4	165.0-166.0	sulfoxide	12.30	17.85	23.48	19.19	14.26	20.43
Peak 5	167.5-168.5	sulfone	30.82	42.58	33.90	40.62	52.37	31.13
a: QX; b: QX-H₂O₂; c: QX-H₂O₂-[Bmim]Br; d: QX-H₂O₂-[Bmim]BF₄; e: QX-H₂O₂-[Bmim]HSO₄; f: QX-H₂O₂-[Bmim]H₂PO₄

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