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光稳定剂中间体2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪的合成研究
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Abstract:
采用单因素法,以三聚氯氰、N-丁基-2,2,6,6-四甲基-4-哌啶胺和氢氧化钠为原料,二甲苯为溶剂,四丁基溴化铵为催化剂合成光稳定剂中间体2-氯-4,6-二(N-丁基-2,2,6,6-四甲基-4-哌啶胺基)-1,3,5-三嗪。结果表明该反应的最优工艺条件为第一阶段反应温度为5℃~8℃,反应时间2 h,第二阶段升温至60℃,反应时间5 h,原料物质的量之比n(三聚氯氰):n(N-丁基-2,2,6,6-四甲基-4-哌啶胺):n(氢氧化钠) = 1:2.15:2.15,催化剂四丁基溴化铵的用量0.20 g (相对0.05 mol三聚氯氰),产品产率为95.61%。
The light stabilizer intermediate 2-chloro-4,6-bis(n-butyl-2,2,6,6-tetramethyl-4-piperidinyl)-1,3,5- triazine was synthesized by single factor method with cyanuric chloride, n-butyl-2,2,6,6-tetra- me-thyl-4-piperidinyl and sodium hydroxide as raw materials, xylene as solvent and tetrabutyl ammo-nium bromide as catalyst. The results showed that the optimum reaction conditions were as follows: the reaction temperature in the first stage was 5?C~8?C, the reaction time was 2 h, the temperature in the second stage was raised to 60?C, the reaction time was 5 h, the ratio of raw material n(cyanuric chloride):n(n-butyl-2,2,6,6-tetramethyl-4-piperidine):n(sodium hydroxide) = 1:2.15:2.15, the amount of catalyst tetrabutyl ammonium bromide was 0.20 g (relative to 0.05 mol cyanuric chloride), the yield of the product was 95.61%.
[1] | 张平安. 受阻胺类光稳定剂的合成及工业化生产[D]: [硕士学位论文]. 广州: 华南理工大学, 2016. |
[2] | Yin, X.P., Zhang, J., Zhang, Z., et al. (2017) Tailoring the Desired Optical and Mechanical Performance of Polyester-Plasticized PVC Films: The Role of Different Light Stabilizers on the Photo-Degradation. Polymers for Advanced Technologies, 28, 1831-1841. https://doi.org/10.1002/pat.4069 |
[3] | 胡应喜, 刘霞, 陈赤阳. 受阻胺光稳定剂的开发研究进展[J]. 北京石油化工学院学报, 2004(2): 15-22. |
[4] | Ryohei, S., Yagi, M., Nozomi, O.F., et al. (2018) Photophysical Properties of Diethylhexyl 2,6-Naphthalate (Corapan TQ), a Photostabilizer for Sunscreens. Photochemical & Photobiological Sciences: Official Journal of the European Photochemistry Association and the European Society for Photobiology, 18, 1556-1564. |
[5] | Zhang, G.H., Zheng, H., Guo, M.Y., et al. (2016) A Novel Polymeric Fluorescent Brightener Agent Based on 4,4’-Diamino-Stilbene-2,2’-Disulfonic Acid-Triazine Structure: Synthesis, Characterization, Photo-Property, and Performance on Paper as Light Stabilizer, Fluorescent Brightener, and Surface-Sizing Agent. Journal of Wood Science, 62, 526-536. https://doi.org/10.1007/s10086-016-1580-5 |
[6] | 姜泽, 鲍芃丞, 李效军, 等. 缚酸剂对合成光稳定剂944中间体4,6-二氯-2-叔辛基氨基-1,3,5-三嗪的影响[J]. 精细石油化工, 2018, 35(1): 5-8. |
[7] | 李惠萍, 蒋登高, 张建华, 等. 光稳定剂中间体2-氯-4,6-二(2,2,6,6-四甲基-4-哌啶氧基)-1,3,5-三嗪的制备[J]. 郑州大学学报(工学版), 2002(2): 20-22. |