CN111234645A - 一种矿用喷涂堵漏风材料及其制备方法 - Google Patents
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Abstract
本发明公开了一种矿用喷涂堵漏风材料及其制备方法,由0.01%—0.03%的氢氧化钠、15%—20%的脲素、20%—30%的甲醛和50%—60%的苯酚充分搅拌混匀混合制成酚脲醛树脂,之后在一定量树脂中按比例加入增韧剂、发泡剂、固化剂等,在常温下均匀搅拌20 s制备高分子泡沫。本发明合成了抗压强度高、弯曲性能好的低成本发泡树脂,泡孔为闭孔结构,堵漏风效果显著,非常适合煤矿井下的漏风治理,能有效防治煤炭自燃、瓦斯积聚等问题。
Description
技术领域
本发明涉及矿井堵漏风材料领域,具体涉及一种矿用喷涂堵漏风材料及其制备方法。
背景技术
矿井漏风不仅是矿井通风工作的重大隐患,也是导致采空区遗煤自燃的重要原因。而矿井裂缝是矿井井下钻探过程中普遍存在的问题,可能造成卡钻、喷孔等其他众多复杂情况和重大事故,对井下钻孔工作危害极大。随着人们对材料性能与结构的进一步认识,材料在人们日常生活中的作用日益凸显。密闭堵漏材料一方面应用在各种建筑物(包括桥体、高铁、居民楼等)裂缝和地下水裂缝通道的封堵;另一方面的应用是在矿井漏风点的堵漏,减少向采空区漏风,防止漏风点瓦斯涌出和煤层自然发火;还可以应用密封堵漏材料增加矿井密闭墙的强度,防止风流短路,确保工作面的通风安全,保证矿井的安全生产。矿井用堵漏材料矿井防漏堵漏中不可或缺的一种材料,堵漏材料性能的优劣决定了矿井防漏堵漏的成功率。目前,使用高分子材料用于采空区的喷涂堵漏已经成为防治漏风的主要手段。高分子泡沫相比水泥砂浆等传统材料具有操作简单、固化时间可调、气密性好、粘结强度高等优势。然而树脂发泡后都存在强度和韧性较差的缺陷。一般提高发泡树脂韧性的方法有两种:一种是通过物理方法加入各种改性的天然橡胶、丁晴橡胶、聚乙烯醇、聚乙二醇、环氧树脂等;另一种是化学方法,通过在发泡树脂的大分子链上引入柔性基团等,如腰果油、桐油、麻油等。酚脲醛(PUF)泡沫是在PUF树脂中加入一定量的固化剂、表面活性剂和发泡剂等助剂,搅拌发泡而成。制成的PUF泡沫既有酚醛泡沫难燃、耐热的优点,也因为尿素的加入适当降低了生产成本。但是这种材料依然存在脆性大、易粉化等缺点,因此PUF泡沫的增韧改性研究具有重大的意义。
发明内容
针对上述现有技术存在的缺陷,本发明提供一种矿用喷涂堵漏风材料及其制备方法。
为实现上述目的,本发明采用的技术方案为:
本发明提供了一种矿用喷涂堵漏风材料,将0.01%—0.03%的氢氧化钠、15%—20%的脲素、20%—30%的甲醛和50%—60%的苯酚充分搅拌混匀混合制成酚脲醛树脂,然后在所述酚脲醛树脂中按所占树脂质量的百分比加入增韧剂3%—8%、发泡剂8%—16%、固化剂15%—18%,表面活性剂6%—12%等,在常温下均匀搅拌20 s制备成矿用喷涂堵漏风材料。
进一步地,所述增韧剂由腰果壳油和硼酸改性的PEG600-BA组合而成,所述发泡剂为氢氟烃,所述固化剂对甲苯磺酸,所述表面活性剂为吐温80。
本发明还提供了上述矿用喷涂堵漏风材料的制备方法,包括以下步骤:
(1)将所述苯酚晶体在烧杯中加热熔化,加热温度为43℃;
(2)把所述甲醛、所述脲素和催化剂按固定比例加入,搅拌均匀后在恒温水浴加热锅中加热2-4h,控制反应温度65℃,冷却至室温制得所述酚脲醛树脂;
(3)按一定的摩尔比n(PEG)/n(BA)=2:1,在250 mL三颈瓶中加入PEG600和BA,在温度上升至110~150℃时,在烧瓶中加入一定量的二甲苯,然后在减压下开始反应,当水分离器中没有分离层时,反应停止,在真空下蒸馏除去残留的二甲苯,最后制得硼酸改性的聚乙二醇;
(4)在室温条件下,把制得的硼酸改性的聚乙二醇、腰果壳油和发泡剂、固化剂、表面活性剂按比例混合均匀,制成酚脲醛发泡树脂的添加剂体系;
(5)在室温条件下,把混合好的添加剂加入树脂中,均匀搅拌20s左右,制得韧性较好的矿用喷涂堵漏风材料。
进一步地,所述矿用喷涂堵漏风材料应用于煤矿井下的堵漏风。
本发明的矿用喷涂堵漏风材料具有以下优势:
材料的发泡时间可调,粘结性强,可以比较方便的喷涂于煤体或隔风墙上;
材料发泡倍数高,生产成本低,抗静电,阻燃性和热稳定性好;
硼酸改性的聚乙二醇和腰果壳油混合用于增韧泡沫,使得材料具备较高的抗压强度和较好的弯曲性能,并且这种材料的井下施工过程中发泡时间可调,粘结性好,泡孔闭合率高,堵漏风效果显著;
材料发泡之后的泡孔闭合率高,在井下使用后,堵漏风效果非常好。
具体实施方式
下面通过对各实施例的描述,对本发明的具体实施方式作进一步详细的说明。显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明中的实施例,本领域技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明保护的范围。
结合以下实施例介绍矿用喷涂堵漏风材料的制备及其发泡试验研究:
(1)把恒温水浴锅温度调至43℃,取苯酚47.05g,放入烧杯内加热融化;
(2)取甲醛26.25g,脲素1.5g,氢氧化钠1g混合均匀后倒入融化的苯酚中;
(3)在65℃条件下加热2-4h后,制得酚脲醛树脂,冷却至室温备用;
(4)按实验室方法制备硼酸改性的聚乙二醇(PEG-BAE);
(5)取硼酸改性的聚乙二醇(PEG-BAE)2g,腰果壳油3g,对甲苯磺酸15g,吐温-80 12g,氢氟烃8g,添加入100g树脂中均匀搅拌20s,倒入模具中发泡成型。
粉化率测试:
粉化率用摩擦后泡沫的重量损失来表示,裁出标准样品(50mm×50mm×50mm),称量M1,然后恒定压力下用砂纸来回打磨30次,称量M2,粉化率的计算公式为:Mf= [(M1-M2)/M1] ×100%,Mf一粉化率,%;M1一原试样总质量,g;M2一实验后试样总质量,g。
力学性能测试:
根据GB/T 20974-2014,用电子万能试验机测试泡沫的抗压强度,试验所用试样为50mm×50mm×50m。在这项测试中,每个数据至少用三个样本进行测试,获得平均值。
表观密度测试:
泡沫的密度根据尺寸和重量来确定。
综合热分析实验:
采用HCT-2 综合热分析仪测定复合材料的热失重(TG)性能,氮气流速30 mL /min,升温速度 10 ℃ /min,升温范围 40 ~900 ℃,样品量为 5 mg 左右。
综合测试结果如表1所示:
表1
参数 | 添加增韧剂 | 不加增韧剂 |
发泡温度(℃) | 58 | 60 |
粉化率(%) | 6 | 28 |
抗压强度(Mpa) | 0.15 | 0.08 |
表观密度(g/cm<sup>3</sup>) | 0.11 | 0.07 |
800℃残余物质量(%) | 46.5 | 51.8 |
由表1可以看出,增韧剂的引入能显著增强泡沫的韧性,相比不添加增韧剂的泡沫,本申请制备的高分子泡沫的发泡温度略微降低,粉化率仅为6%,表观密度和抗压强度分别提高到0.11g/cm3和150kPa,热分析结果显示在高温条件下的热稳定性排序为:纯PUF泡沫>腰果壳油>聚乙烯醇,但增韧剂的引入并未对其热稳定性造成显著影响。
以上所述仅为本发明的一些实施例而已,并不用于限制本发明,对于本领域的技术人员来说,本发明可以有各种更改和变化。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (4)
1.一种矿用喷涂堵漏风材料,其特征在于,将0.01%—0.03%的氢氧化钠、15%—20%的脲素、20%—30%的甲醛和50%—60%的苯酚充分搅拌混匀混合制成酚脲醛树脂,然后在所述酚脲醛树脂中按所占树脂质量的百分比加入增韧剂3%—8%、发泡剂8%—16%、固化剂15%—18%,表面活性剂6%—12%等,在常温下均匀搅拌20 s制备成矿用喷涂堵漏风材料。
2.根据权利要求1所述的一种矿用喷涂堵漏风材料,其特征在于,所述增韧剂由腰果壳油和硼酸改性的PEG600-BA组合而成,所述发泡剂为氢氟烃,所述固化剂对甲苯磺酸,所述表面活性剂为吐温80。
3.一种权利要求1所述的矿用喷涂堵漏风材料的制备方法,其特征在于,包括以下步骤:
(1)将所述苯酚晶体在烧杯中加热熔化,加热温度为43℃;
(2)把所述甲醛、所述脲素和催化剂按固定比例加入,搅拌均匀后在恒温水浴加热锅中加热2-4h,控制反应温度65℃,冷却至室温制得所述酚脲醛树脂;
(3)按一定的摩尔比n(PEG)/n(BA)=2:1,在250 mL三颈瓶中加入PEG600和BA,在温度上升至110~150℃时,在烧瓶中加入一定量的二甲苯,然后在减压下开始反应,当水分离器中没有分离层时,反应停止,在真空下蒸馏除去残留的二甲苯,最后制得硼酸改性的聚乙二醇;
(4)在室温条件下,把制得的硼酸改性的聚乙二醇、腰果壳油和发泡剂、固化剂、表面活性剂按比例混合均匀,制成酚脲醛发泡树脂的添加剂体系;
(5)在室温条件下,把混合好的添加剂加入树脂中,均匀搅拌20s左右,制得韧性较好的矿用喷涂堵漏风材料。
4.根据权利要求1所述的一种矿用喷涂堵漏风材料,其特征在于,所述矿用喷涂堵漏风材料应用于煤矿井下的堵漏风。
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