CN116394360B - 一种木材复合阻燃剂及其制备方法和制备得到的阻燃木材 - Google Patents
一种木材复合阻燃剂及其制备方法和制备得到的阻燃木材 Download PDFInfo
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Classifications
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- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/007—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process employing compositions comprising nanoparticles
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
- B27K3/02—Processes; Apparatus
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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- B27K3/00—Impregnating wood, e.g. impregnation pretreatment, for example puncturing; Wood impregnation aids not directly involved in the impregnation process
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- B27—WORKING OR PRESERVING WOOD OR SIMILAR MATERIAL; NAILING OR STAPLING MACHINES IN GENERAL
- B27K—PROCESSES, APPARATUS OR SELECTION OF SUBSTANCES FOR IMPREGNATING, STAINING, DYEING, BLEACHING OF WOOD OR SIMILAR MATERIALS, OR TREATING OF WOOD OR SIMILAR MATERIALS WITH PERMEANT LIQUIDS, NOT OTHERWISE PROVIDED FOR; CHEMICAL OR PHYSICAL TREATMENT OF CORK, CANE, REED, STRAW OR SIMILAR MATERIALS
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- B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
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Abstract
本发明属于防火材料制备技术领域，具体涉及一种木材复合阻燃剂及其制备方法和制备得到的阻燃木材。所述复合阻燃剂是由1份碱木质素、0.1～0.2份氧化碳纳米角、1份碳酸钾溶于95～98份去离子水中构成的悬乳液。将木材脱去木质素后在所述复合阻燃剂中真空浸渍即得到所需的阻燃木材。本发明制备的阻燃木材不仅阻燃效果好，而且燃烧过程中抑烟无毒，同时加工和制备都易实现。本发明提供的木材复合阻燃剂及利用其制备的阻燃木材均具有广阔的应用前景。
Description
技术领域
本发明属于防火材料制备技术领域，具体涉及一种基于碳纳米材料的木材复合阻燃剂及其制备方法和制备得到的阻燃木材。
背景技术
木材作为可再生资源得到全世界的关注，被广泛应用于建筑、家具和装饰中，与我们的日常生活息息相关。但木材的可燃性易腐蚀性是限制其在室内使用的主要原因，经常被认为是主要的火灾危险，木材燃烧过程中释放的烟雾和有毒气体不仅会降低现场可见度妨碍消防人员的救援和灭火，也是造成火灾中人员伤亡的主要原因。木材的阻燃的研究受到科研人员的关注。
目前已有将阻燃抑烟改性剂添加到木材中，来达到阻燃效果的技术提出，具体应用比较广泛的阻燃剂有：卤素、氮和含磷化合物等有机涂料；硼酸盐、氧化锌、镁铝层状双氢氧化物等无机涂料；还有碳纳米材料涂料。但每种阻燃剂都还或多或少存在阻燃效果不好、烟气较多、产生有害气体等缺陷，另外部分阻燃剂在实验技术或产业化规模上难以实现，不能广泛应用。
因此，开发出一种阻燃效果好，抑烟低毒，容易实现的阻燃木材，具有必要意义。
发明内容
为了解决上述技术问题，本发明目的之一在于提供一种基于碳纳米材料的木材复合阻燃剂及相应制备方法。
本发明采用了以下技术方案：
一种木材复合阻燃剂，该复合阻燃剂是由1份碱木质素、0.1～0.2份氧化碳纳米角、1份碳酸钾溶于95～98份去离子水中构成的悬乳液。
上述木材复合阻燃剂的制备方法，包括以下步骤：
S1.氧化碳纳米角：将碳纳米角按照1g:1000mL的比例加入7.0mol/L稀硝酸中，在30℃的条件下加热氧化回流30～40min，自然冷却至室温后用真空抽滤，再用去离子水清洗至pH为中性，放在室温条件下干燥；
S2.复合阻燃剂：质量比1:1称取碱木质素和碳酸钾加入盛有去离子水的烧杯中进行第一次超声分散，然后加入占碱木质素质量10～20％的S1中制备的氧化碳纳米角混合均匀，进行第二次超声分散，得到所需的木材复合阻燃剂。
优选的，所述步骤S2中，两次超声分散的条件均为：在温度30℃的条件下超声处理30～40min，超声频率为20KHz。
本发明目的之二在于提供一种利用上述木材复合阻燃剂制备的阻燃木材。该阻燃木材的制备方法包括以下步骤：
步骤1.待加工木材干燥后浸入80～85℃亚氯酸钠溶液中4～6h，脱去木质素；
步骤2.脱去木质素的木材浸入木材复合阻燃剂中，-0.1MPa低真空下浸渍6～8h，然后40℃温度下真空干燥，得到所需的阻燃木材。
优选的，步骤1中，木材干燥方法为：将木材置于103℃烘箱中干燥12h。
优选的，步骤S2中，脱去木质素的木材在浸入木材复合阻燃剂前，还经过第二次干燥，第二次干燥的条件为：将木材放入85℃烘箱中干燥8～10h。
优选的，步骤1中，所述亚氯酸钠溶液为pH值4～4.6、质量分数4～6％的亚氯酸钠溶液。
本发明还提供一种由上述木材复合阻燃剂真空浸渍得到的阻燃木材或上述制备方法制备得到的阻燃木材，所述阻燃木材表面及至少100μm深度内均匀分布阻燃剂，所述阻燃剂由碱木质素、氧化碳纳米角和碳酸钾组成。
本发明的有益效果在于：
本发明通过碱木质素、氧化碳纳米角和碳酸钾复配得到木材复合阻燃剂，碱木质素的加入可以阻止碳纳米角的聚集，使碳纳米角分散均匀，并且碱木质素本身也有一定的阻燃效果。碳酸钾是一种传统无机盐阻燃剂，用于木材阻燃，不产生有毒气体、价格低廉、烟产量少，但其添加量高容易诱发木材腐蚀，降低木材机械性能。碳纳米材料作为阻燃添加剂添加少量就可以达到很好的阻燃效果，而且碳纳米角的添加可与无机盐产生协同作用，有益于提高木材的阻燃效果。
利用木材复合阻燃剂制备阻燃木材，首先利用亚氯酸钠脱去木材中的木质素，扩大木材孔径，为阻燃剂的渗入提供途径。再以碱木质素、碳酸钾为原料，惨杂氧化过后的碳纳米角，超声分散后真空浸渍渗入木材内部，燃烧过程中在细胞内部形成炭层，发挥阻隔效果，阻碍可燃气体和氧气进一步进入木材和释放。本发明制备的阻燃木材不仅阻燃效果好，而且燃烧过程中抑烟无毒，同时加工和制备都易实现。本发明提供的木材复合阻燃剂及利用其制备的阻燃木材都具有广阔的应用前景。
附图说明
图1为本发明制备的阻燃木材径向截面的SEM图；
图2为本发明制备的阻燃木材燃烧前后的SEM图，其中a1(200倍)、a2(1000倍)为阻燃木材燃烧前的SEM图，b1(100倍)、b2(1500倍)为燃烧后残炭的SEM图；
图3为实施例1中各组木材的HRR结果图；
图4为实施例1中各组木材的THR结果图；
图5为实施例1中各组木材的TSP结果图；
图6为实施例1中各组木材的COP结果图。
具体实施方式
下面结合实施例对本发明技术方案做出更为具体的说明。
利用基于碳纳米材料的木材复合阻燃剂制备阻燃木材的方法如下：
本实施例所用木材为杉木
1.制备基于碳纳米材料的木材复合阻燃剂
S1.氧化碳纳米角：将0.5g碳纳米角加入500ml的7.0mol/L稀硝酸，在30℃的条件下加热氧化回流30～40min，自然冷却至室温后用小孔径滤膜真空抽滤，用去离子水清洗至pH为中性，放在室温条件下干燥24h；
S2.复合阻燃剂：称取1g碱木质素和1g碳酸钾加入盛有去离子水的烧杯中进行超声分散，然后称取0.1～0.2g步骤S1制备的碳纳米角，边搅拌边缓慢加入烧杯中使其充分混合均匀；最后在频率20KHz，温度30℃的条件下超声分散30～40min，得到所需的木材复合阻燃剂。
2.制备阻燃木材
S3.预处理木材，将木材边角打磨光滑，在103℃的烘箱中干燥12h；
S4.使用亚氯酸钠固体配置4～6％的亚氯酸钠溶液，并用乙酸调节pH值为4.6；将干燥过的木材放入亚氯酸钠溶液中80～85℃加热4～6h，脱去木块中的木质素；
S5.木材放入85℃烘箱中干燥8～10h后，将干燥木材浸入上述木材复合阻燃剂中，-0.1MPa低真空下浸渍6～8h，然后放入40℃的真空干燥器中最终干燥，得到所需的阻燃木材。
实施例1
1.制备木材复合阻燃剂
S1.氧化碳纳米角：将0.5g碳纳米角加入500ml的7.0mol/L稀硝酸，在30℃的条件下加热氧化回流35min，自然冷却至室温后用小孔径滤膜真空抽滤，用去离子水清洗至pH为中性，放在室温条件下干燥24h；
S2.复合阻燃剂：称取1g碱木质素和1g碳酸钾加入盛有去离子水的烧杯中进行超声分散，然后称取0.15g步骤S1制备的碳纳米角，边搅拌边缓慢加入烧杯中使其充分混合均匀；最后在频率20KHz，温度30℃的条件下超声分散35min，得到所需的木材复合阻燃剂。
2.制备阻燃木材
S3.预处理木材，将木材边角打磨光滑，在103℃的烘箱中干燥12h；
S4.使用亚氯酸钠固体配置4％的亚氯酸钠溶液，并用乙酸调节pH值为4.6；将干燥过的木材放入亚氯酸钠溶液中85℃加热6h，脱去木块中的木质素；
S5.脱去木质素的木材放入85℃烘箱中干燥8～10h后，将木材浸入上述木材复合阻燃剂中，-0.1MPa低真空下浸渍8h，然后放入40℃的真空干燥器中最终干燥，得到所需的阻燃木材。
对阻燃木材进行电镜分析，图1是制备的阻燃木材的径向截面图，可以看出复合阻燃剂渗透进木材内部，且有100μm以上的深度，图中圈示部分也可以看到木材内部分布有少量阻燃剂。如图2所示，a1、a2为阻燃木材燃烧前的SEM图，可以看出，复合阻燃剂在木材表面分布均匀；b1、b2为燃烧后残炭的SEM图，发现木材燃烧后表面形成一定厚度的均匀炭层，该炭层可以减少热量和氧气的传递，以此达到阻燃的效果。
对实施例中制备的阻燃木材的阻燃性能进行测试，并与其它几种木材进行对比，结果如图3-图6所示，图中Natural wood表示未脱木质素处理未加复合阻燃剂的杉木样品，Delig-wood表示经过脱木质素处理后的杉木样品，Natural wood/SWCNHs表示未脱木质素处理然后经过复合阻燃剂浸渍的杉木样品，Delig-wood/SWCNHs表示通过脱木质素处理后浸渍复合阻燃剂的杉木样品。
通过锥形量热实验结果显示，Natural wood/SWCNHs的烟雾总产量(TSP)、一氧化碳产生速率(COP)等各项数据相较未添加阻燃剂的原木有小幅度下降。而Delig-wood/SWCNHs组的杉木在燃烧过程中第一个最大热释放速率pk1-HRR和第二个最大热释放速率pk2-HRR较原木的峰值分别下降了37.59％和25.07％，总放热量(THR)下降了55.71％，烟雾总产量(TSP)下降59.81％，并且一氧化碳产生速率(COP)明显下降，达到74.02％。因此可以看出，原木添加复合阻燃剂后阻燃效果有小幅度提升，而脱木质素后再添加复合阻燃剂的木材，放热速率下降，总放热量变少，烟雾释放量明显下降，尤其是一氧化碳释放量减少明显，表明其阻燃效果优异，有希望在减少火灾中人员伤亡等方面发挥作用。
以上实施方式仅用以说明本发明的技术方案，而并非对本发明的限制；尽管参照前述实施方式对本发明进行了详细的说明，本领域的普通技术人员应当理解：凡在本发明创造的精神和原则之内所作的任何修改、等同替换和改进等，均应包含在本发明创造的保护范围之内。
Claims (5)
1.一种阻燃木材的制备方法，其特征在于，包括以下步骤：
步骤1. 待加工木材干燥后浸入80~85℃亚氯酸钠溶液中4~6 h，脱去木质素；
步骤2. 脱去木质素的木材浸入木材复合阻燃剂中，-0.1MPa低真空下浸渍6~8 h，然后40℃温度下真空干燥，得到所需的阻燃木材；
该复合阻燃剂是由1份碱木质素、0.1~0.2份氧化碳纳米角、1份碳酸钾溶于95~98份去离子水中构成的悬乳液；
所述复合阻燃剂的制备方法包括以下步骤：
S1. 氧化碳纳米角：将碳纳米角按照1g:1000mL的比例加入7.0 mol/L稀硝酸中，在30℃的条件下加热氧化回流30~40 min，自然冷却至室温后用真空抽滤，再用去离子水清洗至pH为中性，放在室温条件下干燥；
S2. 复合阻燃剂：质量比1:1称取碱木质素和碳酸钾加入盛有去离子水的烧杯中进行第一次超声分散，然后加入占碱木质素质量10~20%的S1中制备的氧化碳纳米角混合均匀，进行第二次超声分散，得到所需的木材复合阻燃剂；两次超声分散的条件均为：在温度30℃的条件下超声处理30~40 min，超声频率为20KHz。
2.如权利要求1所述的一种阻燃木材的制备方法，其特征在于，步骤1中，木材干燥方法为：将木材置于103℃烘箱中干燥12 h。
3.如权利要求1所述的一种阻燃木材的制备方法，其特征在于，步骤2中，脱去木质素的木材在浸入木材复合阻燃剂前，还经过第二次干燥，第二次干燥的条件为：将木材放入85℃烘箱中干燥8~10 h。
4.如权利要求1所述的一种阻燃木材的制备方法，其特征在于，步骤1中，所述亚氯酸钠溶液为pH值4~4.6、质量分数4~6%的亚氯酸钠溶液。
5.一种使用如权利要求1所述的方法制备得到的阻燃木材，其特征在于，所述阻燃木材表面及至少100 μm深度内均匀分布阻燃剂。
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