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1.青岛科技大学 化工学院,青岛 266042
2.青岛科技大学 化学与分子工程学院,青岛 266042
黄梅(1993—),女,硕士研究生,主要从事精细化学品合成及化工工艺的研究;
*刘福胜,教授,主要从事精细化学品合成及废旧聚合物化学回用研究。E-mail:liufusheng63@sina.com;
宋修艳,副教授,主要从事有机合成及废聚物再资源化的研究。E-mail:xiuyansong@126.com.
纸质出版日期:2018-02-20,
收稿日期:2017-05-26,
修回日期:2017-11-11,
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黄梅, 刘福胜, 宋修艳, 宋湛谦. 废尼龙66醇解制备己二酸二甲酯[J]. 高分子通报, 2018,31(2):59-65.
Mei HUANG, Fu-sheng LIU, Xiu-yan SONG, Zhan-qian SONG. Preparation of Dimethyl Adipate by Alcoholysis of Waste Nylon 66[J]. Polymer Bulletin, 2018,31(2):59-65.
黄梅, 刘福胜, 宋修艳, 宋湛谦. 废尼龙66醇解制备己二酸二甲酯[J]. 高分子通报, 2018,31(2):59-65. DOI: 10.14028/j.cnki.1003-3726.2018.02.008.
Mei HUANG, Fu-sheng LIU, Xiu-yan SONG, Zhan-qian SONG. Preparation of Dimethyl Adipate by Alcoholysis of Waste Nylon 66[J]. Polymer Bulletin, 2018,31(2):59-65. DOI: 10.14028/j.cnki.1003-3726.2018.02.008.
以浓硫酸为催化剂,对尼龙66(PA66)甲醇醇解反应进行了研究。采用红外光谱(FT-IR)和核磁共振技术(
1
H NMR)对醇解产物进行了表征,并确认醇解产物为己二酸二甲酯(DMA)和己二胺(HMD)。采用 L
9
(3
4
)正交实验方法,考察了反应温度、反应时间、催化剂用量及甲醇用量等因素对醇解反应结果的影响,并获得较佳工艺条件为:PA66和硫酸的摩尔比1:2;PA66和甲醇的摩尔比1:20;反应温度为120℃;反应时间为 5h。在此工艺条件下,PA66转化率为100%,DMA和HMD的收率分别达到86. 04%和88. 62%。
The methanolysis of nylon 66 (PA66) was investigated using concentrated sulfuric acid (H
2
SO
) as a catalyst. The structures of the products were characterized by FT-IR and
H NMR
and the results showed that the obtained products are dimethyl adipate (DMA) and hexamethylene diamine (HMD)
respectively. Using L
) orthogonal experiment
the effects of temperature
time
H
dosage and methanol dosage on the methanolysis reaction were studied. And the optimum reaction conditions were obtained: the molar ratio of PA66 to H
is 1:2
the molar ratio of PA66 to methanol is 1:20
reaction temperature is 120℃
reaction time is 5h. Under these conditions
the conversion of PA66 was 100%
the yields of DMA and HMD were reached to 86. 04% and 88. 62%
respectively.
尼龙66醇解己二酸二甲酯己二胺
Nylon 66AlcoholysisDimethyl adipateHexamethylene diamine
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