生物基本征型阻燃环氧树脂的制备及其性能研究

doi:10.3969/j.issn.0253-2417.2022.01.010

摘要/Abstract

摘要：

以香草酸、间二苯酚和表氯醇为原料，采用简单两步法合成了环氧单体1, 3, 3’-三环氧乙烷-2’-甲氧基-二苯甲酮(DEBP)，并进一步和4，4-二氨基二苯砜(DDS)加热混合固化制得对应的环氧树脂DEBP/DDS，与常用的双酚A型环氧树脂(DGEBA)的DDS固化进行对比。研究结果表明：DEBP单体具有比DGEBA单体更高的固化活性。DEBP/DDS环氧树脂的玻璃化转变温度为183℃，也高于DGEBA/DDS树脂。DEBP/DDS环氧树脂机械性能更为优越，弯曲模量和弯曲强度分别为2 437.8和98.6 MPa，拉伸模量和拉伸强度分别为2 523.4和71.1 MPa，均高于DGEBA/DDS环氧树脂。DEBP/DDS环氧树脂表现出更好的阻燃性能，在800℃的残炭量达到了35%，极限氧指数(LOI)达到34%，垂直燃烧等级为UL-94 V-0，总释放热仅为17.8 kJ/g。在不引进任何阻燃元素的情况下，由生物基原料合成了有很大潜力的本征型阻燃环氧树脂。

关键词: 生物基材料, 环氧树脂, 本征型阻燃, 二苯甲酮

Abstract:

The epoxy monomer 1, 3, 3'-tri-oxirane-2'-methoxy-benzophenone(DEBP) was synthesized with vanillic acid, m-diphenol, epichlorohydrin and so on as raw materials by simple two-step method. And DEBP was structurally characterized and determined via FT-IR, and was then mixed with 4, 4'-diaminodiphenylsulfone(DDS), followed by heating and curing to obtain DEBP/DDS epoxy resin. For comparative purpose, commercially used diglycidyl ether of bisphenol A(DGEBA) was cured with the identical curing agent was used as a control. The results showed that DEBP monomer had higher curing activity than that of DGEBA monomer. The glass transition temperature of DEBP/DDS epoxy resin was 183℃, which was higher than that of DGEBA/DDS. The DEBP/DDS epoxy resin outperformed DGEBA/DDS epoxy resin in terms of flexural and tensile properties. The flexural modulus and strength of DEBP/DDS epoxy resin were measured as 2 437.8 and 98.6 MPa and the tensile modulus and strength of DEBP/DDS were 2 523.4 and 71.1 MPa. The cured DEBP/DDS also demonstrated excellent flame retardant property. The char residue at 800℃ reached 35%, the limiting oxygen index(LOI) was 34%, the UL 94 level was V-0 and the total heat release was measured as 17.8 kJ/g. This research suggested that without indroducing any flame retardant element, an intrinsic flame-retarding epoxy resin was synthesized with bio materials.

Key words: biomaterials, epoxy resin, intrinsic flame retardance, benzophenone

中图分类号:

TQ35

潘政, 李卓, 薄采颖, 冯国东, 杨晓慧, 胡立红. 生物基本征型阻燃环氧树脂的制备及其性能研究[J]. 林产化学与工业, 2022, 42(1): 71-78.

Zheng PAN, Zhuo LI, Caiying BO, Guodong FENG, Xiaohui YANG, Lihong HU. Preparation and Performance of Bio-based Intrinsic Flame-retarding Epoxy Resin[J]. Chemistry and Industry of Forest Products, 2022, 42(1): 71-78.

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环氧树脂 epoxy resin	弯曲模量/MPa flexural modulus	弯曲强度/MPa flexural strength	拉伸模量/MPa tensile modulus	拉伸强度/MPa tensile strength
DEBP/DDS	2437.8	98.6	2523.4	71.1
DGEBA/DDS	2313.5	93.7	2132.7	68.7

环氧树脂 epoxy resin	UL 94		LOI/%	峰值时间/s peak time	最大热释放速率/(W·g^-1) peak heat release rate	总释放热/(kJ·g^-1) total heat release
环氧树脂 epoxy resin	熔滴droplet	级别rating	LOI/%	峰值时间/s peak time	最大热释放速率/(W·g^-1) peak heat release rate	总释放热/(kJ·g^-1) total heat release
DEBP/DDS	否no	V-0	34.0	329	186.6	17.8
DGEBA/DDS	是yes	无级别no rating	18.4	303	437.7	25.1

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