松香改性聚硅氧烷阻燃剂的制备及应用研究

doi:10.3969/j.issn.0253-2417.2022.02.010

Abstract

Abstract:

In order to enhance the flame retardancy of polysiloxane, a novel flame retardant rosin grafted polysiloxane(RGSO) was synthesized by the amidation reaction of rosin and amino-polysiloxane. The synthesized flame retardant was employed as a part of the soft segment to produce flame-retarding rigid polyurethane foam(RPUF) by "one-pot" process. The flame retardant rigid polyurethane foams(RPUF-1-RPUF-4) were obtained with the rosin amounts of 5, 10, 15 and 20 g. The structure of the flame retardants was characterized by FT-IR and Py-GC/MS. The microstructure, thermal stability, flame retardant property and compressive strength of the RPUFS were analyzed. The results showed that the hydrogenated phenanthrene ring structure of rosin inhibited the gas release of cyclosioxane and promoted the compactness of the silica-rich carbon layer, and invested the materials with excellent flame retardant since it become shielding layer coated on the substrate surface and effectively insulated thermal and oxygen flame retardant. Compared with unmodified RPUF(P-RPUF), the limited oxygen index(LOI) value of the modified sample(RPUF-3) increased by 37.1%, and the peak heat release rate(PHRR) of the modified sample decreased by 44.8%. The fire growth rate(FIGRA) of the modified materials decreased from 10.99 kW/(m²·s) to 4.33 kW/(m²·s), which indicated that the introduction of RGSO could significantly enhance the flame retardant performance of RPUF. Meanwhile, the rigid hydrogenated phenanthrene ring structure of rosin improved the compressive strength of the modified RPUF. The compressive strength of RPUF-4 was 366.7 kPa, which was higher than that of S-RPUF(112.5 kPa).

Key words: flame retardancy, siloxane, rosin, polyurethane foam

CLC Number:

TQ35

Zhen HUANG, Shibo WANG, Chunyu REN, He LIU, Xu XU, Zhanqian SONG. Preparation and Application of Rosin Modified Siloxane-based Flame Retardant[J]. Chemistry and Industry of Forest Products, 2022, 42(2): 71-79.

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References 17

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样品 sample	MTASO/g	松香/g rosin	黏度/(mPa·s) viscosity
RGSO-1	45	5	6500
RGSO-2	40	10	6650
RGSO-3	35	15	6710
RGSO-4	30	20	6800

编号 No.	主要产物 main product	相对峰面积relative peak area/%
编号 No.	主要产物 main product	MTASO	RGSO-3
1	D₃	6.51	6.22
2	D₄	31.02	41.96
3	D₅	28.28	17.98
4	D₆	18.46	9.07
5	D₇	8.18	3.81
6	D₉	1.91	1.42

样品 sample	阻燃剂 flame retardant	初始热分解温度/℃ initial decomposition temp.	最大热失重速率温度/℃ the maximum loss ratio temp.	最大热失重速率/(%·min^-1) the maximum loss ratio	残渣率(800 ℃)/% residual
P-RPUF	无no	286.4	326.4	5.86	2.1
S-RPUF	MTASO	272.2	327.2	5.33	5.3
RPUF-3	RGSO-3	275.1	330.1	3.61	9.4

样品 sample	最大热释放速率/(kW·m^-2) peak heat release rate(PHRR)	总热释放量/(MJ·m^-2) total heat release(THR)	达到最大热释放速率时间/s time to peak heat release rate(T-PHRR)	火焰蔓延速率/(kW·m^-2·s^-1) fire growth rate(FIGRA)
P-RPUF	274.68	42.89	25	10.99
S-RPUF	232.07	42.18	25	9.28
RPUF-3	151.55	40.93	35	4.33

样品 sample	密度/(kg·m^-3) density	压缩强度/MPa compressive strength	比压缩强度/(kN·m·kg^-1) specific compressive strength	水接触角/° water contact angle
P-RPUF	58.0	0.3310	5.71	115.6
S-RPUF	58.3	0.1125	1.93	130.5
RPUF-1	58.4	0.2105	3.60	129.6
RPUF-2	58.4	0.2756	4.72	127.5
RPUF-3	58.6	0.3248	5.54	126.7
RPUF-4	58.7	0.3667	6.25	126.1

Preparation and Application of Rosin Modified Siloxane-based Flame Retardant

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