糠醛渣分级转化制备分散剂和吸水性树脂

doi:10.3969/j.issn.0253-2417.2023.02.011

摘要/Abstract

摘要：

采用分级转化策略，首先将糠醛渣中的木质素组分制备成木质素基分散剂(LS)，在糠醛渣用量100 g、去离子水用量1 000 g，反应温度70 ℃、反应时间3 h、氢氧化钠用量6.5 g、亚硫酸钠1.6 g、甲醛0.2 g的条件下得到的木质素基分散剂的分散力为105%。以分离得到的纤维素残渣制备吸水性树脂，探究了反应温度、引发剂过硫酸铵(APS)用量、交联剂N，N'-亚甲基双丙烯酰胺(MBA)用量、复合单体丙烯酸(AA)和丙烯酰胺(AM)总用量对吸水性树脂吸水倍率的影响。在丙烯酸中和度为60%，引发时间0.5 h，复合单体用量9 g，引发剂用量1.3 g，交联剂用量0.05 g，反应温度52 ℃，接枝共聚反应时间3 h的优化条件下，吸水性树脂的吸水倍率达到64.6 g/g。FT-IR分析表明AM、AA和纤维素残渣发生了接枝反应；SEM表明反应生成了交联网状结构的产物；热重分析说明AA和AM的引入提高了吸水性树脂的热稳定性；XRD表明AA、AM的接枝反应发生在纤维素残渣的骨架上。

关键词: 糠醛渣, 分级转化, 分散剂, 吸水性树脂

Abstract:

Using the staged conversion strategy, the lignin component in furfural residue(FR) was first prepared into lignin-based dispersant(LS). When the mass of FR was 100 g, the mass of the deionized water was 1 000 g, the reaction temperature was 70℃, the reaction time was 3 h, the dosage of sodium hydroxide was 6.5 g, sodium sulfite dosage was 1.6 g, and formaldehyde dosage was 0.2 g, the dispersing force of LS was 105%. Subsequently, water absorption resin was further prepared from the separated cellulose residue. The effects of the reaction temperature, the amount of initiator ammonium sulfate(APS), crosslinking agent N, N'-methylene bisacrylamide(MBA) and the total amount of complex monomer acrylic acid(AA) and acrylamide(AM) on the water absorption of the water-absorbing resin were investigated. Under the optimum conditions of the neutralization degree of acrylic acid of 60%, the initiation time of 0.5 h, the amount of complex monomer of 9 g, the amount of initiator of 1.3 g, crosslinking agent dosage of 0.05 g, the reaction temperature of 52℃, and the graft copolymerization reaction time of 3 h, the water absorption of the water absorbent resin reached 64.6 g/g. FT-IR analysis showed that the grafting reaction of AM, AA and cellulose residue occurred. SEM images showed that theproduct with cross-linked network structure was formed in the reaction; thermogravimetric analysis showed that the introduction of AA and AM improved the thermal stability of the water absorbent resin; XRD revealed that the grafting reaction of AA and AM took place on the skeleton of cellulose residue.

Key words: furfural residue, staged conversion, dispersant, water absorption resin

中图分类号:

TQ35

桂港, 王小茹, 张璐, 杜朝军, 陈玮, 常春. 糠醛渣分级转化制备分散剂和吸水性树脂[J]. 林产化学与工业, 2023, 43(2): 80-88.

Gang GUI, Xiaoru WANG, Lu ZHANG, Chaojun DU, Wei CHEN, Chun CHANG. Preparation of Dispersant and Water Absorption Resin by Staged Conversion from Furfural Residue[J]. Chemistry and Industry of Forest Products, 2023, 43(2): 80-88.

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样品 sample	分散力/% dispersion forces
LS	105
SQDL-1	100
SQDL-3	104

编号 No.	A 反应温度/℃ reaction temperature	B 复合单体用量/g complex monomer dosage	C 交联剂质量/g crosslinking agent dosage	D 引发剂质量/g initiator dosage	吸水倍率/(g·g^-1) water absorption rate
1	48	7	0.04	1.3	35.0
2	48	8	0.05	1.5	40.2
3	48	9	0.06	1.7	35.3
4	50	7	0.05	1.7	27.5
5	50	8	0.06	1.3	37.6
6	50	9	0.04	1.5	39.9
7	52	7	0.06	1.5	30.9
8	52	8	0.04	1.7	34.9
9	52	9	0.05	1.3	46.9
k₁	36.8	31.1	36.6	39.8
k₂	35.0	37.6	38.2	37.0
k₃	37.6	40.7	34.6	32.6
R	2.6	9.6	3.6	7.2

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