WO2020186903A1 - 一种木材/纳米LDHs阻燃材料及其制备方法 - Google Patents

一种木材/纳米LDHs阻燃材料及其制备方法 Download PDF

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WO2020186903A1
WO2020186903A1 PCT/CN2020/070676 CN2020070676W WO2020186903A1 WO 2020186903 A1 WO2020186903 A1 WO 2020186903A1 CN 2020070676 W CN2020070676 W CN 2020070676W WO 2020186903 A1 WO2020186903 A1 WO 2020186903A1
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wood
ldhs
nano
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flame
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李海龙
公昊
刘梦茹
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South China University of Technology SCUT
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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
    • B27K3/52—Impregnating agents containing mixtures of inorganic and organic compounds
    • 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
    • B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
    • 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
    • B27K2240/00—Purpose of the treatment
    • B27K2240/30—Fireproofing

Definitions

  • the invention relates to the technical field of wood fire-retardant, in particular to a preparation method of wood/nano LDHs fire-retardant material.
  • Wood is a porous, layered, anisotropic heterogeneous natural polymer composite material, which is widely used in many fields such as construction, decoration, and furniture.
  • wood fiber raw material wood is easy to burn and is considered It is a material that is easy to cause fire or spread fire quickly, and has an important impact on the occurrence and development of fire. In order to reduce fires and protect the safety of people's lives and properties, the state has required the use of fire-retardant wood products in public places.
  • Nano flame retardant is a block, film, multilayer film and fiber formed by agglomeration of ultrafine flame retardant particles with a particle size of 1-100nm.
  • the traditional inorganic flame-retardant materials are ultra-fine, and the quantum size effect, small size effect, and surface effect of the nanoparticle itself are used to enhance the interface effect, improve the compatibility of the inorganic substance and the polymer matrix, and reduce the amount and
  • the application of nanotechnology in flame retardant materials has opened up a new field for flame retardant technology.
  • currently existing flame retardants have the problems of large amount and low flame retardant efficiency.
  • the invention provides a wood/nano LDHs flame retardant material and a preparation method.
  • the wood has more and larger pores after being oxidized, and the nano LDHs particles are grown or filled in situ by using a hydrothermal synthesis method or a physical filling method In the wood channel, a wood/nano-LDHs composite material with flame retardant effect is obtained.
  • a preparation method of wood/nano LDHs flame retardant material including the following steps:
  • the porous wood obtained in step (1) is soaked in a metal salt solution and then added to an alkali solution, reacted at 50-150°C for at least 3 hours, washed, and dried to obtain wood with nano-LDHs grown in situ in the pores;
  • the porous wood obtained in step (1) is immersed in the nano-LDHs suspension, the content of the nano-LDHs in the suspension is 0.1-10wt%, stirred for at least 3h, then washed and dried to obtain the pores filled with nano-LDHs wood.
  • the reaction temperature is 60-140°C, and the reaction time is 8-120 h.
  • the content of nano-LDHs in the suspension is 2-5 wt%.
  • the alkaline solution is urea, ammonia, strong alkali and weak acid salt;
  • the types of nano-LDHs include Ni-Al type, Mg-Al type, Zn-Al type, Mn-Al type , Ni-Fe type, Mg-Fe type, Zn-Fe type, Mn-Fe type.
  • the metal salt solution is Ni 2+ -Al 3+ , Mg 2+ -Al 3+ , Zn 2+ -Al 3+ , Mn 2+ -Al 3+ , Ni 2+ -Fe 3+ , Mg 2+ -Fe 3+ , Zn 2+ -Fe 3+ , Mn 2+ -Fe 3+ solution
  • the porous wood is immersed in the metal salt solution for 1-24 hours.
  • the wood raw materials include conifers and hardwoods; the drying temperature is 10 to 120° C., and the drying time is 1 to 24 hours.
  • the oxidation treatment includes the oxidation treatment of ClO 2 , NaClO 2 , K 2 FeO 4 , CH 3 COOOH or NaOH-Na 2 SO 3 .
  • step (2) it is characterized in that, in step (2), the stirring rate is 200-1500 rpm, the stirring temperature is 10-80° C., and the stirring time is 6-48 h.
  • the drying temperature is 10 to 80° C.
  • the drying time is 8 to 48 hours.
  • the present invention provides a wood/nano LDHs flame-retardant material and a preparation method thereof to obtain a wood/nano LDHs composite material with a flame retardant effect.
  • the wood/nano LDHs composite material is prepared by the above preparation method.
  • the wood is oxidized to remove part of the lignin in the intercellular layer, and the pores are enlarged and increased to obtain porous wood.
  • the present invention adopts a hydrothermal synthesis method or a physical filling method to grow or fill nano-LDHs particles in situ in the wood pores. , A wood/nano-LDHs composite material with flame retardant effect is obtained. Since the particles of the flame retardant LDHs are nano-sized, the filling amount of the flame retardant will be greatly reduced, and the flame retardant efficiency will be doubled.
  • the wood in the present invention is a natural porous material, and after simple oxidation treatment, wood with more different pore sizes can be obtained.
  • the nano-LDHs in the present invention have the advantages of large specific surface area (20-250m 2 /g), simple synthesis, low cost, reusable, and no corrosive gas.
  • the nano-LDHs particles are grown in situ or filled in the wood pores and distributed uniformly.
  • the LDHs particles are nano-level, which reduces the amount of flame retardant and has high flame retardant efficiency.
  • Figures 1a and 1b are SEM images of different sections of the pine wood after oxidation treatment in Example 1.
  • Example 2 is the SEM images of the wood/nano-LDHs flame-retardant material prepared in Example 1 at different magnifications.
  • Example 3 is the SEM images of the wood/nano-LDHs flame retardant material prepared in Example 2 at different magnifications.
  • the pine wood was oxidized with NaClO 2 , washed to neutrality, and dried at 80°C for 12 hours to obtain oxidized porous wood. After oxidation, the porous wood was stirred in a suspension of Ni-Al nano-LDHs. The content of LDHs in the suspension was 2wt%, the stirring rate was 800rpm, the stirring temperature was room temperature, and the stirring time was 12h. After washing, it was dried at 50°C for 24h to obtain Wood filled with nano-LDHs in the channels.
  • the obtained scanning electron micrographs of the pine wood after oxidation treatment with NaClO 2 at different magnifications are shown in Figure 1a and Figure 1b.
  • Figure 1a and Figure 1b Through Figure 1a and Figure 1b, the morphology of the cross section and longitudinal section of the wood can be clearly seen, and the pores The diameter is 15-25 ⁇ m, neatly arranged.
  • the obtained scanning electron micrographs of the wood filled with Ni-Al nano-LDHs in the pores at different magnifications are shown in Fig. 2.
  • the Ni-Al LDHs are all nanometers and are evenly distributed in the wood pores.
  • the wood/nano-LDHs composite material has a combustion heat of 8.7kJ/g, and has a flame retardant effect.
  • the eucalyptus was oxidized with K 2 FeO 4 , washed to neutrality, and dried at 120°C for 1 hour to obtain oxidized porous wood. After the oxidized porous wood was soaked in Mg 2+ -Al 3+ metal salt solution for 12 hours, urea solution was added, reacted at 100°C for 48 hours, washed and dried at 60°C for 24 hours to obtain wood with nano-LDHs grown in the pores.
  • the obtained wood with Mg-Al type nano-LDHs grown in the pores after oxidation treatment with K 2 FeO 4 under different magnifications is shown in Figure 3.
  • the Mg-Al type LDHs are all nanometers, and the wood pores Evenly distributed in the road.
  • the wood/nano-LDHs composite material has a combustion heat of 7.9kJ/g and has a flame retardant effect.
  • the obtained wood has Mg-Fe type nano-LDHs grown in the pores after being oxidized by NaOH-Na 2 SO 3 , and the Mg-Fe type LDHs are all nanometers and are evenly distributed in the wood pores.
  • the wood/nano LDHs composite material has a flame retardant effect.
  • the cedar was oxidized with CH 3 COOOH, washed to neutrality, and dried at room temperature for 24 hours to obtain oxidized porous wood. After oxidation, the porous wood is stirred in the Zn-Fe nano-LDHs suspension.
  • the content of LDHs in the suspension is 5wt%
  • the stirring rate is 500rpm
  • the stirring temperature is 50°C
  • the stirring time is 48h
  • it is dried at 80°C for 8h
  • the obtained wood is filled with Zn-Fe type nano-LDHs in the pores after the CH 3 COOOH oxidation treatment, and the Zn-Fe type LDHs are all nanometers and are evenly distributed in the wood pores.
  • the wood/nano LDHs composite material has a flame retardant effect.

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Wood Science & Technology (AREA)
  • Forests & Forestry (AREA)
  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical And Physical Treatments For Wood And The Like (AREA)

Abstract

一种木材/纳米LDHs阻燃材料及其制备方法，包括如下步骤：(1)对木材原料进行氧化处理，洗涤至中性，干燥，得到氧化后多孔木材；(2)采取水热合成法或者物理填充法制备木材/纳米LDHs阻燃材料，将纳米LDHs颗粒原位生长或填充在木材孔道中，得到具有阻燃效果的木材/纳米LDHs复合材料。该方法操作简单，成本低廉。纳米LDHs在木材孔道中均匀分布，得到具有阻燃效果的木材/纳米LDHs复合材料。该材料可广泛用于建筑、家居装饰、化工产品等方面。

Description

一种木材/纳米LDHs阻燃材料及其制备方法 技术领域
本发明涉及木材阻燃技术领域，具体涉及一种木材/纳米LDHs阻燃材料的制备方法。
背景技术
木材是一种多孔状、层次状、各向异性的非均质天然高分子复合材料，被广泛应用于建筑、装潢、家具等许多领域，而木材作为一种木质纤维原料，易燃烧，被认为是一种容易引起火灾或使火灾迅速蔓延的材料，对火灾的发生及发展具有重要的影响。为了减少火灾保障人民生命财产安全，国家已要求在公共场合必须使用阻燃处理的木制品。
纳米阻燃剂是由颗粒尺寸为l～100nm的超微阻燃粒子凝聚而成的块体、薄膜、多层膜和纤维。将传统的无机阻燃材料超细化，利用纳米微粒本身所具有的量子尺寸效应、小尺寸效应、表面效应来增强界面作用，改善无机物和聚合物基体的相容性，达到减小用量和提高阻燃性的目的，纳米技术在阻燃材料中的应用为阻燃技术开辟了一个新的领域。然而，目前现有阻燃剂存在用量大，且阻燃效率不高的问题。
发明内容
本发明提供了一种木材/纳米LDHs阻燃材料及制备方法，木材经氧化处理后具有更多、更大的孔道，利用水热合成法或物理填充法，将纳米LDHs颗粒原位生长或填充在木材孔道中，得到具有阻燃效果的木材/纳米LDHs复合材料。
本发明的目的通过如下技术方案实现：
一种木材/纳米LDHs阻燃材料的制备方法，包括如下步骤：
(1)对木材进行预处理
对木材原料进行氧化处理，洗涤至中性，干燥，得到氧化后多孔木材；
(2)采取如下任意一种方法制备木材/纳米LDHs阻燃材料
水热合成法：将步骤(1)中得到的多孔木材经金属盐溶液浸泡后加入碱溶液，50～150℃反应至少3h后洗涤，干燥，得到孔道内原位生长了纳米LDHs的木材；
物理填充法：将步骤(1)中得到的多孔木材浸泡于纳米LDHs悬浮液中，悬浮液中纳米LDHs含量为0.1～10wt％，搅拌至少3h后洗涤，干燥，得到孔道内填充了纳米LDHs的木材。
优选地，步骤(2)中，反应温度为60～140℃，反应时间为8～120h。
优选地，步骤(2)中，悬浮液中纳米LDHs含量为2～5wt％。
优选地，步骤(2)中，所述碱溶液为尿素、氨水、强碱弱酸盐；所述纳米LDHs的种类包括Ni-Al型、Mg-Al型、Zn-Al型、Mn-Al型、Ni-Fe型、Mg-Fe型、Zn-Fe型、Mn-Fe型。
优选地，步骤(2)中，所述金属盐溶液为Ni 2+-Al 3+、Mg 2+-Al 3+、Zn 2+-Al 3+、Mn 2+-Al 3+、Ni 2+-Fe 3+、Mg 2+-Fe 3+、Zn 2+-Fe 3+、Mn 2+-Fe 3+溶液，所述孔木材经金属盐溶液浸泡的时间为1～24h。
优选地，步骤(1)中，所述木材原料包括针叶木、阔叶木；所述干燥温度为10～120℃，干燥时间为1～24h。
优选地，步骤(1)中，所述氧化处理包括选用ClO 2、NaClO 2、K 2FeO 4、CH 3COOOH或NaOH-Na 2SO 3氧化处理。
优选地，其特征在于，步骤(2)中，所述搅拌速率为200～1500rpm，搅拌温度为10～80℃，搅拌时间为6～48h。
优选地，步骤(2)中，水热合成法和物理填充法中，所述干燥温度为10～80℃，干燥时间为8～48h。
本发明提供了一种木材/纳米LDHs阻燃材料及制备方法，得到具有阻燃 效果的木材/纳米LDHs复合材料，所述木材/纳米LDHs复合材料由以上制备方法制备。木材经过氧化处理脱除胞间层中部分木素，使孔道增大、增多，得到多孔木材，本发明采用水热合成法或物理填充法，将纳米LDHs颗粒原位生长或填充在木材孔道中，得到具有阻燃效果的木材/纳米LDHs复合材料，由于阻燃剂LDHs的颗粒为纳米级，阻燃剂的填充量将会大大减少，阻燃效率将会加倍提高。
本发明具有如下优点和有益效果：
(1)本发明中木材作为一种天然多孔材料，经过简单的氧化处理，即可得到具有更多不同孔径的木材。
(2)本发明中纳米LDHs具有比表面积大(20～250m 2/g)、合成简单、成本低廉、可重复利用、不产生腐蚀性气体的优点。
(3)本发明中纳米LDHs颗粒原位生长或填充在木材孔道中，分布均匀，LDHs颗粒为纳米级，减少了阻燃剂的用量，阻燃效率高。
(4)得到具有阻燃效果的木材/纳米LDHs复合材料，可广泛用于建筑、家居装饰、化工产品等人类生活的各个方面，无二次污染。
附图说明
图1a和图1b为实施例1中氧化处理后的松木不同切面的SEM图。
图2为实施例1中制备的木材/纳米LDHs阻燃材料不同倍率的SEM图。
图3为实施例2中制备的木材/纳米LDHs阻燃材料不同倍率的SEM图。
具体实施方式
以下结合具体实施例及附图对本发明技术方案作进一步地详细的说明，但本发明的保护范围不仅限于此。
实施例1
使用NaClO 2对松木进行氧化处理，洗涤至中性，在80℃下干燥12h，得到氧化后多孔木材。氧化后多孔木材在Ni-Al型纳米LDHs悬浮液中搅拌，悬浮液中LDHs含量为2wt％，搅拌速率为800rpm，搅拌温度为室温，搅拌时间 为12h，洗涤后在50℃下干燥24h，得到在孔道内填充纳米LDHs的木材。
得到的经NaClO 2氧化处理后的松木在不同倍率下的扫描电镜图如图1a和图1b所示，通过图1a和图1b可清晰地看到木材中横截面和纵切面的形貌，孔道直径为15-25μm，排列整齐。得到的在孔道内填充Ni-Al型纳米LDHs的木材在不同倍率下的扫描电镜图如图2所示，Ni-Al型LDHs均为纳米级，在木材孔道内分布均匀。该木材/纳米LDHs复合材料的燃烧热为8.7kJ/g，具有阻燃效果。
实施例2
使用K 2FeO 4对桉木进行氧化处理，洗涤至中性，在120℃下干燥1h，得到氧化后多孔木材。氧化后多孔木材经Mg 2+-Al 3+金属盐溶液浸泡12h后，加入尿素溶液，在100℃下反应48h，洗涤后在60℃下干燥24h，得到在孔道内生长纳米LDHs的木材。
得到的经K 2FeO 4氧化处理后在孔道内生长了Mg-Al型纳米LDHs的木材在不同倍率下的扫描电镜图如图3所示，Mg-Al型LDHs均为纳米级，在木材孔道内分布均匀。该木材/纳米LDHs复合材料的燃烧热为7.9kJ/g，具有阻燃效果。
实施例3
使用NaOH-Na 2SO 3对杨木进行氧化处理，洗涤至中性，在50℃下干燥16h，得到氧化后多孔木材。氧化后多孔木材经Mg 2+-Fe 3+金属盐溶液浸泡24h后，加入氨水溶液，在60℃下反应120h，洗涤后在室温下干燥48h，得到在孔道内生长纳米LDHs的木材。
得到的经NaOH-Na 2SO 3氧化处理后在孔道内生长了Mg-Fe型纳米LDHs的木材，Mg-Fe型LDHs均为纳米级，在木材孔道内分布均匀。该木材/纳米LDHs复合材料具有阻燃效果。
实施例4
使用CH 3COOOH对杉木进行氧化处理，洗涤至中性，在室温下干燥24h， 得到氧化后多孔木材。氧化后多孔木材在Zn-Fe型纳米LDHs悬浮液中搅拌，悬浮液中LDHs含量为5wt％，搅拌速率为500rpm，搅拌温度为50℃，搅拌时间为48h，洗涤后在80℃下干燥8h，得到在孔道内填充纳米LDHs的木材。
得到的经CH 3COOOH氧化处理后在孔道内填充Zn-Fe型纳米LDHs的木材，Zn-Fe型LDHs均为纳米级，在木材孔道内分布均匀。该木材/纳米LDHs复合材料具有阻燃效果。
以上实施例仅为本发明较优的实施方式，仅用于解释本发明，而非限制本发明，本领域技术人员在未脱离本发明精神实质下所作的改变、替换、修饰等均应属于本发明的保护范围。

Claims (10)

  1. 一种木材/纳米LDHs阻燃材料的制备方法，其特征在于，包括如下步骤：
    (1)对木材进行预处理
    对木材原料进行氧化处理，洗涤至中性，干燥，得到氧化后多孔木材；
    (2)采取如下任意一种方法制备木材/纳米LDHs阻燃材料
    水热合成法：将步骤(1)中得到的多孔木材经金属盐溶液浸泡后加入碱溶液，50～150℃反应至少3h后洗涤，干燥，得到孔道内原位生长了纳米LDHs的木材；
    物理填充法：将步骤(1)中得到的多孔木材浸泡于纳米LDHs悬浮液中，悬浮液中纳米LDHs含量为0.1～10wt％，搅拌至少3h后洗涤，干燥，得到孔道内填充了纳米LDHs的木材。
  2. 根据权利要求1所述的方法，其特征在于，步骤(2)中，反应温度为60～140℃，反应时间为8～120h。
  3. 根据权利要求1所述的方法，其特征在于，步骤(2)中，悬浮液中纳米LDHs含量为2～5wt％。
  4. 根据权利要求1或2或3所述的方法，其特征在于，步骤(2)中，所述碱溶液为尿素、氨水、强碱弱酸盐；所述纳米LDHs的种类包括Ni-Al型、Mg-Al型、Zn-Al型、Mn-Al型、Ni-Fe型、Mg-Fe型、Zn-Fe型、Mn-Fe型。
  5. 根据权利要求1或2或3所述的方法，其特征在于，步骤(2)中，所述金属盐溶液为Ni 2+-Al 3+、Mg 2+-Al 3+、Zn 2+-Al 3+、Mn 2+-Al 3+、Ni 2+-Fe 3+、Mg 2+-Fe 3+、Zn 2+-Fe 3+、Mn 2+-Fe 3+溶液，所述孔木材经金属盐溶液浸泡的时间为1～24h。
  6. 根据权利要求1或2或3所述的方法，其特征在于，步骤(1)中，所述木材原料包括针叶木、阔叶木；所述干燥温度为10～120℃，干燥时间为1～24h。
  7. 根据权利要求1或2或3所述的方法，其特征在于，步骤(1)中，所 述氧化处理包括选用ClO 2、NaClO 2、K 2FeO 4、CH 3COOOH或NaOH-Na 2SO 3氧化处理。
  8. 根据权利要求1或2或3所述的方法，其特征在于，步骤(2)中，所述搅拌速率为200～1500rpm，搅拌温度为10～80℃，搅拌时间为6～48h。
  9. 根据权利要求1或2或3所述的方法，其特征在于，步骤(2)中，水热合成法和物理填充法中，所述干燥温度为10～80℃，干燥时间为8～48h。
  10. 权利要求1至9中任意一项所述方法制备的木材/纳米LDHs阻燃材料。
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