温度和气氛对高K高S糠醛渣灰分的烧结特性研究

doi:10.11949/0438-1157.20211237

化工学报 ›› 2022, Vol. 73 ›› Issue (1): 411-424.DOI: 10.11949/0438-1157.20211237

温度和气氛对高K高S糠醛渣灰分的烧结特性研究

王晓蓉¹(),曾玺^2,³(),王芳^2,³,张光义^2,³,许德平¹,许光文^3,⁴

^1.中国矿业大学（北京）化学与环境工程学院，北京 100083
^2.北京工商大学生态环境学院，北京 100048
^3.中国科学院过程工程研究所多相复杂系统国家重点实验室，北京 100190
^4.沈阳化工大学资源化工与材料教育部重点实验室，辽宁沈阳 110142

收稿日期:2021-08-26 修回日期:2021-11-02 出版日期:2022-01-05 发布日期:2022-01-18
通讯作者: 曾玺
作者简介:王晓蓉(1995—)，女，硕士研究生，wangxiaorongjl@163.com
基金资助:
国家重点研发计划项目(2019YFC1906805)

Effect of temperature and atmosphere on ash sintering characteristics of furfural residue with high K and S

Xiaorong WANG¹(),Xi ZENG^2,³(),Fang WANG^2,³,Guangyi ZHANG^2,³,Deping XU¹,Guangwen XU^3,⁴

^1.School of Chemical and Environmental Engineering, China University of Mining and Technology, Beijing 100083, China
^2.School of Ecology and Environment, Beijing Technology and Business University, Beijing 100048, China
^3.State Key Laboratory of Multi-phase Complex Systems, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100190, China
^4.Key Laboratory on Resources of Chemicals and Materials of Ministry of Education, Shenyang University of Chemical Technology, Shenyang 110142, Liaoning, China

Received:2021-08-26 Revised:2021-11-02 Online:2022-01-05 Published:2022-01-18
Contact: Xi ZENG

摘要/Abstract

摘要：

糠醛渣的能源化利用是糠醛产业清洁生产和碳减排的有效途径。然而，现有的直接燃烧利用常面临着因糠醛渣高K引起的灰分烧结严重、高S导致的SO_x排放量大和高水含量导致的燃烧效率低等难题。基于此，在管式炉中考察了单一气氛(N₂、CO₂、O₂)和混合气氛(N₂+H₂O、CO₂+H₂O、O₂+H₂O)中糠醛渣灰在不同温度下的烧结特性，并对灰分颜色、收缩率、微观形貌、矿物质成分和K/S释放等特性进行系统分析。灰分热收缩行为显示，随温度升高，灰样收缩率增加；在单一气氛中添加水蒸气能促进灰分烧结。SEM分析发现，在灰分烧结前，其微观结构在低温下已出现熔融和结渣。XRD分析表明，灰分烧结与低熔点矿物生成紧密相关。单一气氛中，高温下N₂促进钾长石生成；CO₂抑制钾长石生成；O₂促进钙铝黄长石和透辉石生成。在混合气氛中，水蒸气的出现促进多种低熔点钾铝硅酸盐生成，如钾长石和白榴石等。XRF分析显示，随温度升高，灰样中K的固留率(G_K)和S的固留率(G_S)降低；在考察的单一气氛中，高温时，N₂中G_K最低；G_S受气氛的影响较小。在考察的复合气氛中，高温时，G_K受气氛影响较小；G_S受气氛影响严重，特别地，O₂+H₂O气氛中G_S最高，S逸散最少。为抑制糠醛渣灰分烧结和K/S元素逸散到气相中，糠醛渣在流化床燃烧过程中应控制运行温度(低于900℃)、降低气氛中N₂的含量。

关键词: 生物质, 解耦燃烧, 流化床, 碱金属, 烧结, 气氛

Abstract:

The energy utilization of furfural residue is an effective way for clean generation and carbon reduction in furfural industry. However, the existing direct combustion and utilization often face problems such as serious ash sintering caused by high K of furfural slag, large SO_x emissions caused by high S, and low combustion efficiency caused by high water content. To solve these problems, in this study, a tubular furnace was employed to research the sintering behavior of furfural residue ash in the pure (N₂, CO₂, O₂) and mixed (N₂+H₂O, CO₂+H₂O, O₂+H₂O) atmosphere at different temperatures. The variations of ash color, shrinking rate, micromorphology, mineral compositions and K/S release characteristics were systematically analyzed. The results show that with the increase of temperature, the ash sample shrinking rate increased. Steam played important promotion roles in ash sintering. SEM analysis indicated that the ash microstructure was melted and slaged at low temperature before sintering. XRD analysis displayed that ash sintering was closely related to the composition change of ash. N₂ promoted the composition of microcline, CO₂ inhibited the composition of microcline, while O₂ strengthened the formation of anorthite and diopside. Steam promoted the formation of various potassium aluminum silicates such as microcline and leucite. XRF analysis indicated that, with the increase of temperature, G_K(retention rate of K) and G_S(retention rate of S) in ash decreased. In pure atmospheres, G_K was the smallest in N₂, while the effect of pure atmosphere on G_S was limited. In the mixed atmospheres, compared to G_K, the effect of atmospheres on G_S was much more obvious, especially in O₂+H₂O. To restrain ash sintering and migrate K and S, the suitable operating conditions of furfural residue combustion in fluidized bed should be at temperature below 900℃ and lower N₂ content in atmosphere by introducing a stream of flue gas.

Key words: biomass, decoupling combustion, fluidized bed, alkali metal, sintering, atmosphere

中图分类号:

TQ 519

王晓蓉, 曾玺, 王芳, 张光义, 许德平, 许光文. 温度和气氛对高K高S糠醛渣灰分的烧结特性研究[J]. 化工学报, 2022, 73(1): 411-424.

Xiaorong WANG, Xi ZENG, Fang WANG, Guangyi ZHANG, Deping XU, Guangwen XU. Effect of temperature and atmosphere on ash sintering characteristics of furfural residue with high K and S[J]. CIESC Journal, 2022, 73(1): 411-424.

图/表 20

表1 糠醛渣处理技术分析

Table 1 Technology analysis of furfural residue utilization

利用技术	优点	局限性
堆积或填埋	简单，无技术难度	占用大量土地，产生二次污染
作物栽培	提高农作物产量和菌类产菌率	食品安全性有待验证
土壤用肥	提高碱性土壤可耕作性，扩大可耕种土地面积	难进行大规模利用且仅适用于盐碱土地
提取木质素或纤维素	经济效益好	生产成本高，工艺复杂
制备活性炭	工艺比较成熟，设备投资少，生产成本低	活性炭品质低，仅适用于工业污水处理
燃烧等能源化利用	成本低，处理效率快，可为糠醛生产提供热量	原料高含水，燃烧室温度分布不均，灰分易烧结，NO_x含量高

表2 生物质灰中碱金属和硫含量对比

Table 2 Comparison of alkali metal content in biomass ash samples

生物质灰	含量/%(质量)
生物质灰	Na₂O	K₂O	SO₃
糠醛渣	0.94	12.57	23.82
稻壳	0.39	1.86	0.09
木屑	0.01	8.21	7.60
花生壳	0.67	10.40	3.42
谷壳	2.90	0.06	1.3
杨树	8.20	0.70	5.50
稻秸秆	10.80	1.91	2.36

表3 糠醛渣的工业和元素分析

Table 3 Proximate and ultimate analysis of furfural residue

样品	工业分析 w_ad/%				元素分析 w_daf/%
样品	M	A	V	FC	C	H	O^①	N	S
糠醛渣	4.53	20.94	61.68	12.85	56.45	5.66	36.75	0.69	0.45

表4 糠醛渣灰样成分分析

Table 4 Components of furfural residue ash

各种组分含量/%(质量)
SiO₂	SO₃	K₂O	Al₂O₃	CaO	Fe₂O₃	MgO	P₂O₅	TiO₂	其他
37.78	23.82	12.57	9.06	5.79	3.78	3.08	1.72	1.12	1.28

图1 灰分烧结装置示意图1—阀门;2—流量计;3—加热炉;4—瓷舟;5—炉堵;6—刚玉管;7—控制系统

Fig.1 Schematic diagram of experimental system for ash agglomeration

图2 N2和N2+H2O气氛中灰样热处理的形貌(a)及收缩率(b)演变

Fig.2 Variation of ash morphologies (a) and shrinking rate (b) at different temperatures in N2 and N2+H2O

图3 CO2和CO2+H2O气氛中灰样热处理的形貌(a)及收缩率(b)演变

Fig.3 Variation of ash morphologies (a) and shrinking rate (b) at different temperatures in CO2 and CO2+H2O

图4 O2和O2+H2O气氛中灰样热处理的形貌(a)及收缩率(b)演变

Fig.4 Variation of ash morphologies (a) and shrinking rate (b) at different temperatures in O2 and O2+H2O

图5 单一气氛(a)和水蒸气混合气氛(b)中灰样收缩率对比

Fig.5 Variation of shrinking rate at different temperatures in pure (a) and mixed (b) atmosphere

图6 N2 (a)和N2+H2O (b)气氛中灰样热处理的微观形貌

Fig.6 Micro morphology of ash samples at different temperatures in N2 (a) and N2+H2O (b)

图7 CO2 (a)和CO2+H2O (b)气氛中灰样热处理的微观形貌

Fig.7 Micro morphology of ash samples at different temperatures in CO2 (a) and CO2+H2O (b)

图8 O2 (a)和O2+H2O (b)气氛中灰样热处理的微观形貌

Fig.8 Micro morphology of ash samples at different temperatures in O2 (a) and O2+H2O (b)

图9 N2 (a)和N2+H2O (b)气氛中灰样成分演变

Fig.9 Components variation of ash sample in N2 (a) and N2+H2O (b) at different temperatures

表5 各气氛中灰样热处理的典型数据分析

Table 5 Typical data analysis for thermal treatment of biomass ash

气氛		灰样烧结温度区间/℃	烧结前收缩率范围
单一气氛	N₂	1000~1100	30.1~68.9
	CO₂	1100~1150	42.4~55
	O₂	1100~1150	49.3~77.3
混合气氛	N₂+H₂O	900~1000	26.7~57.3
	CO₂+H₂O	1000~1100	35~59.6
	O₂+H₂O	1000~1100	19.3~64

表6 不同气氛中灰样成分

Table 6 Components of ash sample in different atmospheres

序号	化学式	名称	熔融/分解温度℃	序号	化学式	名称	熔融/分解温度℃
1	SiO₂	石英	1750	12	CaSO₄	硫酸钙	880~1150
2	Ca(Al₂SiO₈)	钙长石	1250~1550	13	Fe₂SiO₄	铁橄榄石	1200
3	K(AlSi₃O₈)	钾长石	1130~1450	14	(KH)₂(MgFe)₂(AlFe)₂(SiO₄)	黑云母	1800
4	CaAl₄O₇	钙铝氧化物	1890	15	KAlSi₂O₆	白榴石	1120~1380
5	Mg₂SiO₄	镁橄榄石	1580~1750	16	Ca(Mg,Al,Fe)Si₂O₆	辉石	1300~1400
6	Al₅SiO_9.5	莫来石	1170~1390	17	SiO₂	硫方英石	1713
7	CaMgSi₂O₆	透辉石	2054~2572	18	Ca₃Al₂(SiO₄)₃	钙铝榴石	1080
8	NaAlSiO₄	霞石	1526	19	KAlSi₃O₈	正长石	1050
9	Ca₂Al₂SiO₇	钙铝黄长石	1593	20	NaFeSi₂O₆	锥辉石	1000~1204
10	KAlSiO₄	钾铝硅酸盐	1130~1450	21	(Ca_0.79Fe_0.21)SiO₃	铁硅灰石	1540
11	Al₂(SO₄)₂	硫酸铝	880~1150

图10 CO2 (a)和CO2+H2O (b)气氛中灰样成分演变

Fig.10 Components variation of ash in CO2 (a) and CO2+H2O (b) at different temperatures

图11 O2 (a)和O2+H2O (b)气氛中灰样成分

Fig.11 Components variation of ash in O2 (a) and O2+H2O (b) at different temperatures

图12 单一气氛中热处理灰样中K (a)和S (b)固留率变化

Fig.12 Retention rate variation of K (a) and S (b) in ash samples treated by different pure atmospheres

图13 复合气氛中热处理灰样中K (a)和S (b)固留率变化

Fig.13 Variation of retention rate of K (a) and S (b) in ash samples treated by different mixed atmospheres

表7 糠醛渣灰样在高温下发生的反应

Table 7 Reactions among components in furfural residue ash at high temperatures

序号	化学反应方程式
R1	Al₂(SO₄)₃ $→ ?????$ Al₂O₃＋3SO₃
R2	CaSO₄ $→ ?????$ CaO+SO₃
R3	CaO+Al₂O₃ $→ ?????$ CaAl₄O₇
R4	K₂O+Al₂O₃+6SiO₂ $→ ?????$ 2K(AlSi₃O₈)
R5	2CaO+Al₂O₃+SiO₂ $→ ?????$ Ca₂Al₂SiO₇
R6	10K(AlSi₃O₈)+5SO₃ $→ ?????$ 2Al₅SiO_9.5+28SiO₂+5K₂SO₄
R7	CaO+MgO+2SiO₂ $→ ?????$ CaMgSi₂O₆
R8	Na₂O+Al₂O₃+2SiO₂ $→ ?????$ 2NaAlSiO₄
R9	2MgO+SiO₂ $→ ?????$ Mg₂SiO₄
R10	4FeO+2SiO₂ $→ ?????$ 2Fe₂SiO₄
R11	K₂O+Al₂O₃+2SiO₂ $→ ?????$ 2KAlSiO₄
R12	K₂O+Al₂O₃+4SiO₂ $→ ?????$ 2KAlSi₂O₆
R13	3CaO+Al₂O₃+3SiO₂ $→ ?????$ Ca₃Al₂(SiO₄)₃
R14	Na₂O+Fe₂O₃+4SiO₂ $→ ?????$ 2NaFeSi₂O₆

表7 糠醛渣灰样在高温下发生的反应

Table 7 Reactions among components in furfural residue ash at high temperatures

序号	化学反应方程式
R1	Al₂(SO₄)₃ $→ ?????$ Al₂O₃＋3SO₃
R2	CaSO₄ $→ ?????$ CaO+SO₃
R3	CaO+Al₂O₃ $→ ?????$ CaAl₄O₇
R4	K₂O+Al₂O₃+6SiO₂ $→ ?????$ 2K(AlSi₃O₈)
R5	2CaO+Al₂O₃+SiO₂ $→ ?????$ Ca₂Al₂SiO₇
R6	10K(AlSi₃O₈)+5SO₃ $→ ?????$ 2Al₅SiO_9.5+28SiO₂+5K₂SO₄
R7	CaO+MgO+2SiO₂ $→ ?????$ CaMgSi₂O₆
R8	Na₂O+Al₂O₃+2SiO₂ $→ ?????$ 2NaAlSiO₄
R9	2MgO+SiO₂ $→ ?????$ Mg₂SiO₄
R10	4FeO+2SiO₂ $→ ?????$ 2Fe₂SiO₄
R11	K₂O+Al₂O₃+2SiO₂ $→ ?????$ 2KAlSiO₄
R12	K₂O+Al₂O₃+4SiO₂ $→ ?????$ 2KAlSi₂O₆
R13	3CaO+Al₂O₃+3SiO₂ $→ ?????$ Ca₃Al₂(SiO₄)₃
R14	Na₂O+Fe₂O₃+4SiO₂ $→ ?????$ 2NaFeSi₂O₆

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温度和气氛对高K高S糠醛渣灰分的烧结特性研究

Effect of temperature and atmosphere on ash sintering characteristics of furfural residue with high K and S

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