酚化木质素改性酚醛树脂胶黏剂的制备及性能表征

doi:10.3969/j.issn.0253-2417.2019.06.013

摘要/Abstract

摘要：

在碱性条件下，酸性木质素先经苯酚处理，再用于对酚醛树脂进行改性，制备得到木质素改性酚醛树脂（LPF）胶黏剂，考察了木质素用量、苯酚处理时间及温度、苯酚处理木质素时氢氧化钠水溶液用量（第一批次氢氧化钠）、酚醛物质的量比对LPF胶黏剂性能的影响。研究结果表明：在木质素用量25%、苯酚处理时间2 h、苯酚处理温度80℃、第一批次氢氧化钠水溶液用量8%、苯酚与甲醛的物质的量比1.0：2.0时，LPF胶黏剂的胶合强度为1.57 MPa，较未经改性的酚醛树脂（PF）胶黏剂的1.35 MPa提高了16.3%，游离苯酚为0.58%，比PF的0.72%降低了19.4%，游离甲醛0.16%、固体质量分数51.2%、pH值11.4、黏度80 mPa·s、贮存期为60天。FT-IR分析表明：LPF在2893和1213 cm^-1处吸收峰明显减弱，表明木质素分子中甲氧基部分脱落；在1505、1320、1114和875 cm^-1处吸收峰消失，表明合成酚醛树脂过程中，木质素中的磺酸基消失；在1018 cm^-1处的吸收峰明显增强，表明有新的醚键生成。

关键词: 木质素, 改性, 酚醛树脂, 胶黏剂

Abstract:

A lignin-modified phenol formaldehyde resin adhesive (LPF) was prepared from the modified phenol formaldehyde resin which was treated under alkaline conditions. The performance of LPF was investigated by the dosage of lignin (L), phenol treatment time and temperature, sodium hydroxide (first batch of sodium hydroxide) and phenol/formaldehyde molar ratio (n(P)/n(F)). The results showed that LPF bond was achieved when the content of lignin was 25%, the phenol treatment time was 2 h, the treatment temperature was 80℃, the first batch of sodium hydroxide was 8%, and the phenol/formaldehyde molar ratio was 1.0:2.0. The bond strength is 1.57 MPa, which was 16.3% higher than 1.35 MPa of unmodified phenol formaldehyde adhesive (PF).0.58% of free phenol, which was 19.4% lower than 0.72% of PF.The result also showed of formaldehyde content 0.16%, solid content of 51.2%, pH value of 11.4, viscosity of 80 mPa·s, and storage period of 60 days. FT-IR analysis showed that the absorption peaks of LPF at 2893 and 1213 cm^-1 were obviously weakened, indicating that the methoxy moiety in the lignin molecule was partially shed.The absorption peak disappeared at 1505, 1320, 1114, 875 cm^-1, indicating that most of the sulfonic acid groups in the lignin disappeared during the synthesis of the phenol formaldehyde resin; the absorption peak at 1018 cm^-1 was significantly enhanced, indicating the formation of a new ether bond.

Key words: lignin, modification, phenol formaldehyde resin, adhesive

中图分类号:

TQ35

李宁,陈智糠,张一甫. 酚化木质素改性酚醛树脂胶黏剂的制备及性能表征[J]. 林产化学与工业, 2019, 39(6): 95-101.

Ning LI,Zhikang CHEN,Yifu ZHANG. Preparation and Characterization of Phenol Formaldehyde Resin Adhesives Modified by the Phenolic Lignin[J]. Chemistry and Industry of Forest Products, 2019, 39(6): 95-101.

图/表 4

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样品 sample	胶合强度/MPa bond strength	游离苯酚/% free phenol	游离甲醛/% free formaldehyde	固体质量分数/% solid mass fraction	黏度/(mPa·s) viscosity	pH值 pH value	贮存期/d storage time
PF	1.35	0.72	0.08	45.9	90	12.5	55
LPF	1.57	0.58	0.16	51.2	80	11.4	60
GB/T 14732—2017	≥0.7	≤1.0	≤0.3	≥35	≥60	≥7.0

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