糠醛渣木质素/聚乙烯亚胺微球的制备

doi:10.16085/j.issn.1000-6613.2019-1162

摘要/Abstract

摘要：

木质素和聚乙烯亚胺（PEI）对重金属离子有良好的亲和力，且木质素来源广泛、具有良好的生物降解性能，在水处理方面有很好的前景。本文以糠醛渣木质素和聚乙烯亚胺为主要原料，十二烷基苯磺酸钠（SDBS）为分散剂，环氧氯丙烷（EPI）为交联剂，液体石蜡为油相，采用反相悬浮聚合法，制备了糠醛渣木质素/PEI微球（LMS）。通过FTIR、XRD、SEM和激光粒度仪对微球的结构和形貌进行表征，研究了木质素用量、PEI用量、EPI用量、SDBS用量、油水比和反应温度对木质素微球制备的影响。结果显示，在木质素用量为0.600g，PEI用量为2.25g，EPI用量为2.25mL，SDBS用量为0.075g，温度为56℃，油水体积比为4.5∶1的条件下，制得的糠醛渣木质素/PEI微球平均粒径为135μm，粒径分散度为0.290，比表面积为46.5m²/g，球型度良好，球体表面有少量微孔。

关键词: 糠醛渣木质素, 聚乙烯亚胺, 微球, 制备, 反相悬浮聚合法

Abstract:

Lignin and polyethyleneimine (PEI) have good affinity for heavy metal ions, and lignin sources have a wide range of good biodegradability and good prospects in water treatment. The furfural residue lignin/PEI microspheres (LMS) were prepared with furfural residue lignin and polyethyleneimine by inverse suspension polymerization, which epichlorohydrin (EPI) was used as crosslinked agent, sodium dodecylbenzenesulfonate(SDBS) was of dispersing agent, and liquid paraffin was the oil phase. The structure and morphology of the microspheres were characterized by FTIR, XRD, SEM and laser particle size analyzer. The amount of lignin, the amount of PEI, the amount of crosslinker, the amount of dispersant, the ratio of oil to water and the reaction temperature were studied for lignin micro. The results showed that the optimal conditions for furfural lignin/PEI microspheres preparation were lignin dosages of 0.600g, PEI dosage of 2.25g, EPI dosage of 2.25mL, SDBS dosage of 0.075g, reaction temperature of 56℃, and oil to water volume ratio of 4.5∶1. The obtained lignin microspheres had good spherical shape, uniform particle size, a small amount of potholes on the surface of the sphere and a specific surface area of 46.5m²/g. The average particle diameter was 135μm with uniformity of 0.290.

Key words: furfural residue lignin, polyethyleneimine, microspheres, preparation, inverse suspension polymerization

中图分类号:

TQ317.9

朱春山,毛正鑫,高琳. 糠醛渣木质素/聚乙烯亚胺微球的制备[J]. 化工进展, 2020, 39(4): 1550-1557.

Chunshan ZHU,Zhengxin MAO,Lin GAO. Preparation of furfural residue lignin/poluethyleneimine microspheres[J]. Chemical Industry and Engineering Progress, 2020, 39(4): 1550-1557.

图/表 14

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木质素用量/g	平均粒径/μm				平均粒径标准差
0.400	282	292	284	292	4.68
0.500	191	192	199	207	6.44
0.600	241	251	249	240	5.00
0.700	187	175	175	186	5.49
0.900	181	170	184	168	6.83

木质素用量/g	平均粒径/μm				平均粒径标准差
0.400	282	292	284	292	4.68
0.500	191	192	199	207	6.44
0.600	241	251	249	240	5.00
0.700	187	175	175	186	5.49
0.900	181	170	184	168	6.83

实验水平	温度/℃	PEI/g	木质素/g	交联剂/mL	油水比	分散剂/g
1	56	1.75	0.400	1.50	3.0∶1	0.050
2	60	2.00	0.500	1.75	3.5∶1	0.075
3	64	2.25	0.600	2.00	4.0∶1	0.100
4	68	2.50	0.700	2.25	4.5∶1	0.125
5	72	2.75	0.800	2.50	5.0∶1	0.150

实验水平	温度/℃	PEI/g	木质素/g	交联剂/mL	油水比	分散剂/g
1	56	1.75	0.400	1.50	3.0∶1	0.050
2	60	2.00	0.500	1.75	3.5∶1	0.075
3	64	2.25	0.600	2.00	4.0∶1	0.100
4	68	2.50	0.700	2.25	4.5∶1	0.125
5	72	2.75	0.800	2.50	5.0∶1	0.150

实验号	温度/℃	PEI/g	木质素/g	EPI/mL	油水比	分散剂/g	平均粒径/μm	分散度
1	56	1.75	0.400	1.50	3.0∶1	0.050	188	0.256
2	56	2.00	0.500	1.75	3.5∶1	0.075	182	0.378
3	56	2.25	0.600	2.00	4.0∶1	0.100	131	0.425
4	56	2.50	0.700	2.25	4.5∶1	0.125	127	0.348
5	56	2.75	0.800	2.50	5.0∶1	0.150	149	0.322
6	60	1.75	0.500	2.00	4.5∶1	0.150	266	0.297
7	60	2.00	0.600	2.25	5.0∶1	0.050	132	0.332
8	60	2.25	0.700	2.50	3.0∶1	0.075	176	0.329
9	60	2.50	0.800	1.50	3.5∶1	0.100	184	0.372
10	60	2.75	0.400	1.75	4.0∶1	0.125	227	0.259
11	64	1.75	0.600	2.50	3.5∶1	0.125	213	0.261
12	64	2.00	0.700	1.50	4.0∶1	0.150	238	0.248
13	64	2.25	0.800	1.75	4.5∶1	0.050	150	0.395
14	64	2.50	0.400	2.00	5.0∶1	0.075	211	0.208
15	64	2.75	0.500	2.25	3.0∶1	0.100	207	0.231
16	68	1.75	0.700	1.75	5.0∶1	0.100	264	0.191
17	68	2.00	0.800	2.00	3.0∶1	0.125	251	0.210
18	68	2.25	0.400	2.25	3.5∶1	0.150	208	0.205
19	68	2.50	0.500	2.50	4.0∶1	0.050	376	0.305
20	68	2.75	0.600	1.50	4.5∶1	0.100	226	0.326
21	72	1.75	0.800	2.25	4.0∶1	0.075	208	0.320
22	72	2.00	0.400	2.50	4.5∶1	0.100	181	0.311
23	72	2.25	0.500	1.50	5.0∶1	0.125	214	0.286
24	72	2.50	0.600	1.75	3.0∶1	0.150	178	0.221
25	72	2.75	0.700	2.00	3.5∶1	0.050	170	0.234
均值1	155	228	203	210	200	203	—	—
均值2	197	197	249	200	191	194	—	—
均值3	204	176	176	206	236	199	—	—
均值4	265	215	195	176	190	206	—	—
均值5	190	196	188	219	194	208	—	—
极差	110	52.23	72.73	42.53	45.8	14.0	—	—