盾粉/橡胶阻燃复合材料的制备与性能

赵令; 张浩; 徐维成; 申振伟; 李海丽; 龙红明

盾粉/橡胶阻燃复合材料的制备与性能

赵令¹,
张浩^{1, 2, 3, ,},
徐维成²,
申振伟¹,
李海丽³,
龙红明^{1, 2}

1.
安徽工业大学冶金工程学院, 马鞍山 243032
2.
冶金减排与资源综合利用教育部重点实验室, 马鞍山 243002
3.
安徽工业大学建筑工程学院, 马鞍山 243032

基金项目: 国家自然科学基金(52174290)，安徽省高校协同创新项目(GXXT-2020-072)，安徽省杰青项目(2208085 J19)，中国博士后科学基金(2017 M612051)

详细信息

通讯作者:
张浩，博士，副教授，硕士生导师，研究方向为冶金固废无害高附加值非建材领域利用研究，　E-mail: fengxu19821018@163.com

中图分类号: TB332
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- 文章访问数: 318
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- 被引次数: 0
出版历程
- 收稿日期: 2022-10-11
- 修回日期: 2022-11-02
- 录用日期: 2022-11-12
- 网络出版日期: 2022-12-01

Preparation and properties studies of shield powder/rubber flame retardant composite material

Ling ZHAO¹,
Hao ZHANG^{1, 2, 3
, ,},
Weicheng XU²,
Zhenwei SHEN¹,
Haili LI³,
Hongming LONG^{1, 2}

1.
School of Metallurgical Engineering, Anhui University of Technology, Ma’an shan 243032, China
2.
Anhui Province Key Laboratory of Metallurgy Engineering & Resources Recycling (Anhui University of Technology), Ma’an shan 243002, China
3.
School of Civil Engineering and Architecture, Anhui University of Technology, Ma’an shan, 243032, China

Funds: National Natural Science Foundation of china (No. 52174290); Collaborative Innovation of Universities in Anhui Project (No. GXXT-2020-072); Anhui Jieqing Project (No. 2208085 J19)4; and Postdoctoral Science Foundation of china (No. 2017 M612051)

摘要

摘要: 橡胶复合材料在制备过程中，由于添加炭黑、硫磺等物质，因此往往需要添加一定量的阻燃剂，提高橡胶复合材料的阻燃性能。而钢渣中的铁、硅、镁、铝等金属氧化物是良好的阻燃-消烟剂，将钢渣应用于橡胶中，在减少昂贵阻燃剂用量、提高阻燃性能的同时，也实现冶金大宗固废-钢渣新途径应用，为碳中和与碳达峰贡献微薄力量。本文通过功能助剂对钢渣进行化学改性，得到800目的钢渣粉(盾粉)，并将盾粉应用橡胶中替代氢氧化铝，制备出盾粉/橡胶阻燃复合材料。从图1可以看出，与未替代氢氧化铝(ZL0)相比，ZL1~ZL3的最大烟密度(MSD)与烟密度等级(SDR)均下降；从图2中可以看出，与ZL0相比，ZL1~ZL3的残余率高于ZL0；从表1中可以看出，ZL1~ZL3的水平燃烧与垂直燃烧的燃烧时间均大幅缩短，ZL2、ZL3在水平燃烧时出现自熄现象，导致燃烧速度无法测量，同时氧指数均提高2%。这是因为在燃烧过程中，利用盾粉本身含有Al₂O₃、MgO、SiO₂、Fe₂O₃等物质间形成了具有协同增效作用的阻燃-消烟体系，在橡胶复合材料内部形成一个可以阻挡橡胶内部因高温分解产生的可燃性气体向外挥发，以及阻挡热量和火焰向材料内部传递的致密炭层，在一定程度上减缓盾粉/橡胶阻燃复合材料剧烈燃烧反应的发生。1盾粉/橡胶阻燃复合材料烟密度测试结果2橡胶阻燃复合材料的TG测试结果

1盾粉/橡胶阻燃复合材料燃烧性能测试结果

Sample	Horizontal burning			Vertical burning			氧指数
Sample	Burning time/s	Burning speed(mm/min)	Burning grade	Burning time/s	Phenomenon	Burning grade	Oxygen-index(%)		Materialgrade
ZL0	30	40	HB	18.4	Drip burning	V-2	22	Slow-burning
ZL1	13	27	HB	16.3	Drip burning	V-2	24	Slow-burning
ZL2	9	0	HB	14.4	Drip burning	V-2	24	Slow-burning
ZL3	4	0	HB	13.6	Drip burning	V-2	24	Slow-burning

关键词:

盾粉 /
氢氧化铝 /
橡胶 /
炭渣 /
阻燃性能

Abstract: The functional material (called shield powder) was formed by mixing functional additives with ordinary carbon steel slag under the work of ultra-fine vertical mill, and replaced the flame retardant filler aluminum hydroxide to form shield powder/rubber composite material. In order to reveal the flame retardant mechanism of shield powder in the rubber system, the paper tested vulcanization properties, mechanical properties and combustion properties and analyzed the gas phase and solid phase residues in the combustion process of shield powder/rubber composite material. The results show that, the shield powder prepared from steel slag could promote the vulcanization process of rubber system, shorten vulcanization time and increase vulcanization rate index. What is more, it can replace aluminum hydroxide as flame retardant filler of rubber system and has little effect on mechanical properties. Besides in the combustion process of shield powder/rubber flame retardant composite material, there are Al₂O₃, MgO, SiO₂, Fe₂O₃ and other substances in shield powder to form a synergistic flame retardant-smoke extinguishing system. Furthermore, the main mineral composition of carbon slag of shield powder/rubber flame retardant composite material is ZnS and FeS₂ and is closely related to the proportion of shield powder replacing alumina hydroxide. With the increase of substitution ratio, there are SiO₂ and MnP newly in carbon slag.

Key words:

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图 1 盾粉生产工艺图

Figure 1. Production and technology process of shield powder

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图 2 盾粉/橡胶阻燃复合材料硫化测试结果

Figure 2. Vulcanization results of shield powder / rubber flame retardant composite material

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图 3 盾粉/橡胶阻燃复合材料力学性能测试结果

Figure 3. Mechanical properties results of shield powder / rubber flame retardant composite material

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图 4 盾粉/橡胶阻燃复合材料烟密度测试结果

Figure 4. Smoke density results of shield powder / rubber flame retardant composite material

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图 5 盾粉/橡胶阻燃复合材料的TG测试结果

Figure 5. TG results of shield powder / rubber flame retardant composite material

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图 6 盾粉/橡胶阻燃复合材料炭渣的XRD测试结果

Figure 6. XRD results of shield powder / rubber flame retardant composite material carbon slag

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图 7 盾粉/橡胶阻燃复合材料炭渣的拉曼与SEM测试结果

Figure 7. Raman and SEM results of shield powder / rubber flame retardant composite material carbon slag

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图 8 盾粉/橡胶阻燃复合材料硫化-阻燃机制图

Figure 8. Vulcanization-flame retardant mechanism of shield powder / rubber flame retardant composite material

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1 盾粉/橡胶阻燃复合材料燃烧性能测试结果

Sample	Horizontal burning			Vertical burning			氧指数
Sample	Burning time/s	Burning speed(mm/min)	Burning grade	Burning time/s	Phenomenon	Burning grade	Oxygen-index(%)		Materialgrade
ZL0	30	40	HB	18.4	Drip burning	V-2	22	Slow-burning
ZL1	13	27	HB	16.3	Drip burning	V-2	24	Slow-burning
ZL2	9	0	HB	14.4	Drip burning	V-2	24	Slow-burning
ZL3	4	0	HB	13.6	Drip burning	V-2	24	Slow-burning

下载: 导出CSV

表 1 盾粉的化学成分与粒径分布

Table 1. Chemical composition and particle size distribution of shield powder

Sample	Chemical compositions/wt%									Particle size/µm
Sample	CaO	P₂O₅	SiO₂	Al₂O₃	MgO	Fe₂O₃	MnO	SO₃	Others	d90	d50	d10
Shield powder	38.97	2.06	19.31	4.03	4.21	24.95	3.45	0.86	2.16	10.04	3.80	1.13

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表 2 盾粉/橡胶阻燃复合材料原料配比/g

Table 2. Ratio of shield powder / rubber flame retardant composite material/g

Raw material	RF	SP/RF-1	SP/RF-2	SP/RF-3	SP/RF-4
Milled rubber	100	100	100	100	100
Styrene butadiene rubber(SBR·150)	42.64	42.64	42.64	42.64	42.64
Butadiene rubber(BR·900)	78.35	78.35	78.35	78.35	78.35
Carbon black(N220)	121.64	121.64	121.64	121.64	121.64
Shield powder(800 mesh)	0	5.54	11.09	16.53	22.07
Aluminum hydroxide	22.07	16.53	10.98	5.54	0
70 Chlorinated paraffins	44.24	44.24	44.24	44.24	44.24
Zinc oxide	8.85	8.85	8.85	8.85	8.85
Stearic acid	2.24	2.24	2.24	2.24	2.24
Antideteriorant(4010)	2.24	2.24	2.24	2.24	2.24
Antideteriorant(RD)	3.30	3.30	3.30	3.30	3.30
Antimony oxide	6.61	6.61	6.61	6.61	6.61
Protective wax(L-5866)	4.37	4.37	4.37	4.37	4.37
Sulphur	4.37	4.37	4.37	4.37	4.37
Accelerator(TT)	6.40	6.40	6.40	6.40	6.40
Accelerator(CZ)	2.45	2.45	2.45	2.45	2.45

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表 3 盾粉/橡胶阻燃复合材料燃烧性能测试结果

Table 3. Combustion performance results of shield powder / rubber flame retardant composite material

Sample	Horizontal burning			Vertical burning			Oxygen index
Sample	Burning time/s	Burning speed/ (mm·min⁻¹)	Burning grade	Burning time/s	Phenomenon	Burning grade	Oxygen index/%	Material grade
ZL0	30	40	HB	18.4	Drip burning	V-2	22	Slow-burning
ZL1	13	27	HB	16.3	Drip burning	V-2	24	Slow-burning
ZL2	9	0	HB	14.4	Drip burning	V-2	24	Slow-burning
ZL3	4	0	HB	13.6	Drip burning	V-2	24	Slow-burning

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