CN114350169B - Preparation method of formaldehyde-free high-strength electromagnetic shielding wood fiber composite material - Google Patents
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- 229920002522 Wood fibre Polymers 0.000 title claims abstract description 118
- 239000002025 wood fiber Substances 0.000 title claims abstract description 118
- 239000002131 composite material Substances 0.000 title claims abstract description 47
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- 229920001807 Urea-formaldehyde Polymers 0.000 claims description 11
- GZCGUPFRVQAUEE-SLPGGIOYSA-N aldehydo-D-glucose Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C=O GZCGUPFRVQAUEE-SLPGGIOYSA-N 0.000 claims description 11
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Abstract
本发明涉及木塑复合材料技术领域，且公开了一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：（1）得到改性木质纤维；（2）得到聚乙烯醇溶液；（3）得到中间料；（4）得到木质纤维复合材料；本发明制备的无醛高强度电磁屏蔽的木质纤维复合材料各组分均无游离甲醛，且胶黏剂产品无游离甲醛释放，实现了纤维板的无醛化。
The invention relates to the technical field of wood-plastic composite materials, and discloses a method for preparing a wood fiber composite material without aldehyde and high-strength electromagnetic shielding, comprising the following steps: (1) obtaining modified wood fiber; (2) obtaining polyvinyl alcohol solution; (3) to obtain an intermediate material; (4) to obtain a wood fiber composite material; each component of the aldehyde-free high-strength electromagnetic shielding wood fiber composite material prepared by the present invention has no free formaldehyde, and the adhesive product has no free formaldehyde release , to achieve no formaldehyde of fiberboard.
Description
技术领域technical field
本发明涉及木塑复合材料技术领域，具体为一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法。The invention relates to the technical field of wood-plastic composite materials, in particular to a method for preparing a formaldehyde-free high-strength electromagnetic shielding wood fiber composite material.
背景技术Background technique
纤维板又名密度板，是以木质纤维或其他植物素纤维为原料，施加脲醛树脂或其他适用的胶粘剂制成的人造板。制造过程中可以施加胶黏剂和(或)添加剂。纤维板具有材质均匀、纵横强度差小、不易开裂等优点，用途广泛。制造1立方米纤维板约需2.5～3立方米的木材，可代替3立方米锯材或5立方米原木。发展纤维板生产是木材资源综合利用的有效途径。Fiberboard, also known as density board, is a wood-based panel made of wood fiber or other vegetable fiber and applied with urea-formaldehyde resin or other suitable adhesives. Adhesives and/or additives may be applied during the manufacturing process. Fiberboard has the advantages of uniform material, small vertical and horizontal strength difference, not easy to crack, etc., and has a wide range of uses. It takes about 2.5-3 cubic meters of wood to make 1 cubic meter of fiberboard, which can replace 3 cubic meters of sawn timber or 5 cubic meters of logs. The development of fiberboard production is an effective way to comprehensively utilize wood resources.
在传统的木质纤维人造板材的生产中，板材上压贴所用胶黏剂有大量游离甲醛的释放。随着人们对室内环境要求的提高以及国家相关环保法律法规的出台，木质纤维人造板产品的无醛化迫在眉睫。研究者们针对纤维板的胶粘剂和生产工艺一一的无醛化分别进行了研究。无醛胶黏剂主要包括天然胶黏剂、改性生物基胶黏剂、无醛(改性)高分子树脂胶黏剂等几类。生产工艺上的改进主要以热压工艺为主，微波热压的出现克服了传统热压工艺的众多缺点。In the production of traditional wood fiber-based panels, the adhesive used for pressing and pasting the panels releases a large amount of free formaldehyde. With the improvement of people's requirements for indoor environment and the promulgation of relevant national environmental protection laws and regulations, it is imminent for wood fiber-based panel products to be free of formaldehyde. The researchers conducted research on the non-formaldehyde of the adhesive and the production process of the fiberboard. Formaldehyde-free adhesives mainly include natural adhesives, modified bio-based adhesives, and formaldehyde-free (modified) polymer resin adhesives. The improvement of the production process is mainly based on the hot pressing process. The emergence of microwave hot pressing has overcome many shortcomings of the traditional hot pressing process.
在传统的木质纤维人造板材的生产中，板材上压贴所用胶黏剂有大量游离甲醛的释放。随着人们对室内环境要求的提高以及国家相关环保法律法规的出台，木质纤维人造板产品的无醛化迫在眉睫。研究者们针对纤维板的胶粘剂和生产工艺一一的无醛化分别进行了研究。无醛胶黏剂主要包括天然胶黏剂、改性生物基胶黏剂、无醛(改性)高分子树脂胶黏剂等几类。生产工艺上的改进主要以热压工艺为主，微波热压的出现克服了传统热压工艺的众多缺点。In the production of traditional wood fiber-based panels, the adhesive used for pressing and pasting the panels releases a large amount of free formaldehyde. With the improvement of people's requirements for indoor environment and the promulgation of relevant national environmental protection laws and regulations, it is imminent for wood fiber-based panel products to be free of formaldehyde. The researchers conducted research on the non-formaldehyde of the adhesive and the production process of the fiberboard. Formaldehyde-free adhesives mainly include natural adhesives, modified bio-based adhesives, and formaldehyde-free (modified) polymer resin adhesives. The improvement of the production process is mainly based on the hot pressing process. The emergence of microwave hot pressing has overcome many shortcomings of the traditional hot pressing process.
现有的木质纤维板复合材料性能一般，尤其是在需要电磁屏蔽场合应用中，受到较多的限制。The performance of the existing wood fiberboard composite materials is average, especially in applications where electromagnetic shielding is required, and are subject to more restrictions.
基于此，我们提出了一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，希冀解决现有技术中的不足之处。Based on this, we propose a preparation method of a wood fiber composite material with no formaldehyde and high strength electromagnetic shielding, hoping to solve the deficiencies in the prior art.
发明内容Contents of the invention
(一)解决的技术问题(1) Solved technical problems
针对现有技术的不足，本发明提供了一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法。Aiming at the deficiencies of the prior art, the invention provides a preparation method of a wood fiber composite material with no formaldehyde and high strength electromagnetic shielding.
(二)技术方案(2) Technical solution
为实现上述的目的，本发明提供如下技术方案：To achieve the above object, the present invention provides the following technical solutions:
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
作为进一步的技术方案：所述木质纤维、膨润土分散液混合质量比为1:5；As a further technical scheme: the mixing mass ratio of the wood fiber and bentonite dispersion is 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
作为进一步的技术方案，所述聚乙烯醇溶液质量分数为15％。As a further technical solution, the mass fraction of the polyvinyl alcohol solution is 15%.
作为进一步的技术方案，所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1-2。As a further technical solution, the mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1-2.
作为进一步的技术方案：所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂300-500、纳米吸波剂3-5、羟甲基纤维素30-50、消泡剂3-5、纳米碳酸钙10-15、去离子水100-110。As a further technical solution: the modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 300-500, nano wave absorbing agent 3-5, hydroxymethyl cellulose 30-50, defoamer 3 -5, nano calcium carbonate 10-15, deionized water 100-110.
作为进一步的技术方案：所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1400-1600℃，真空环境下煅烧4h，即得纳米核壳吸波剂；As a further technical solution: the preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, and stir magnetically for 30 minutes , and then carry out centrifugal filtration, wash with ethanol for 3 times, put it in a vacuum drying oven, then add it to a ball mill for ball milling and mixing, and mix for 1 hour; after mixing evenly, move it into a resistance furnace at 1400-1600 ° C under a vacuum environment Calcined for 4 hours to obtain the nano-core-shell absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
作为进一步的技术方案，所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。As a further technical solution, the mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
作为进一步的技术方案，所述硅粉纯度为98％-99.99％，粒度为235-2000目。As a further technical solution, the silicon powder has a purity of 98%-99.99% and a particle size of 235-2000 mesh.
作为进一步的技术方案于，所述消泡剂为有机硅消泡剂。As a further technical solution, the defoamer is a silicone defoamer.
作为进一步的技术方案，所述木质纤维复合材料中改性胶黏剂的施胶量为100-150kg/m3。As a further technical solution, the sizing amount of the modified adhesive in the wood fiber composite material is 100-150 kg/m 3 .
本发明中制备的改性胶黏剂胶合强度高，于木质纤维分子的亲和力较强，从而使得制备的木质纤维复合材料的力学性能得到明显的增加，本发明通过引入纳米吸波剂不仅能够增强了复合材料的电磁屏蔽性能，同时，还能够与脲醛树脂中的游离甲醛发生特定的吸附反应，从而显著的抑制了复合材料的游离甲醛的释放。The modified adhesive prepared in the present invention has high bonding strength and strong affinity to wood fiber molecules, so that the mechanical properties of the prepared wood fiber composite materials are significantly increased. The present invention can not only enhance the The electromagnetic shielding performance of the composite material is improved, and at the same time, it can also have a specific adsorption reaction with the free formaldehyde in the urea-formaldehyde resin, thereby significantly inhibiting the release of the free formaldehyde of the composite material.
(三)有益效果(3) Beneficial effects
与现有技术相比，本发明提供了一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，具备以下有益效果：Compared with the prior art, the present invention provides a method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, which has the following beneficial effects:
本发明制备的无醛高强度电磁屏蔽的木质纤维复合材料各组分均无游离甲醛，且胶黏剂产品无游离甲醛释放，实现了纤维板的无醛化。Each component of the formaldehyde-free high-strength electromagnetic-shielding wood fiber composite material prepared by the invention has no free formaldehyde, and the adhesive product has no free formaldehyde release, so the formaldehyde-free fiberboard is realized.
纳米核壳吸波粒子的引入使得纤维板具备优良的电磁屏蔽性能，可用于重要信息的加密，也可以用于家装，保护人类免受因长期暴露于电磁辐射中的伤害。The introduction of nano-core-shell absorbing particles makes the fiberboard have excellent electromagnetic shielding performance, which can be used for encryption of important information, and can also be used for home decoration to protect human beings from long-term exposure to electromagnetic radiation.
本发明通过对木质纤维的改性处理，能够极大的改善木质纤维的结构性能，在木质纤维结构间隙中插入膨润土粒子，在木质纤维分子链上接枝活性基团，从而不仅能够极大的提高了木质纤维的力学性能，同时，其与胶黏剂之间的结合性能大幅度增加，进而使得制备的木质纤维复合材料的力学性能得到明显的增加。The present invention can greatly improve the structural properties of wood fibers by modifying wood fibers, insert bentonite particles in the gaps of wood fiber structures, and graft active groups on wood fiber molecular chains, thereby not only greatly improving The mechanical properties of the wood fiber are improved, and at the same time, the bonding performance between the wood fiber and the adhesive is greatly increased, so that the mechanical properties of the prepared wood fiber composite material are significantly increased.
附图说明Description of drawings
图1为不同纳米核壳吸波剂添加重量份对电磁屏蔽性能的影响图。Figure 1 is a graph showing the influence of different nano-core-shell absorbers by weight on the electromagnetic shielding performance.
具体实施方式Detailed ways
下面将结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，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，本领域普通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。The following will clearly and completely describe the technical solutions in the embodiments of the present invention with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some, not all, embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by persons of ordinary skill in the art without making creative efforts belong to the protection scope of the present invention.
实施例1Example 1
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1。The mixing mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂300、纳米吸波剂3、羟甲基纤维素30、消泡剂3、纳米碳酸钙10、去离子水100。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 300, nano wave absorbing agent 3, hydroxymethyl
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1400℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then conduct centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1400°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为100kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 100kg/m 3 .
实施例2Example 2
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1.1。The mixing mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1.1.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂350、纳米吸波剂4、羟甲基纤维素35、消泡剂4、纳米碳酸钙11、去离子水102。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 350, nano
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1450℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then conduct centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1450°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为110kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 110kg/m 3 .
实施例3Example 3
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1.2。The mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1.2.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂380、纳米吸波剂3.5、羟甲基纤维素38、消泡剂3.2、纳米碳酸钙12、去离子水104。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 380, nano wave absorbing agent 3.5, hydroxymethyl cellulose 38, defoamer 3.2, nano calcium carbonate 12, deionized water 104.
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1500℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then conduct centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1500°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为120kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 120kg/m 3 .
实施例4Example 4
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1.5。The mixing mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1.5.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂400、纳米吸波剂4、羟甲基纤维素40、消泡剂4、纳米碳酸钙13、去离子水105。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 400, nano
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1500℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorbing agent: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then carry out centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1500°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为120kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 120kg/m 3 .
实施例5Example 5
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:1.6。The mixing mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:1.6.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂450、纳米吸波剂4.5、羟甲基纤维素40、消泡剂4.5、纳米碳酸钙14、去离子水108。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 450, nano wave absorbing agent 4.5, hydroxymethyl
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1550℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then conduct centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1550°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为140kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 140kg/m 3 .
实施例6Example 6
一种无醛高强度电磁屏蔽的木质纤维复合材料的制备方法，包括以下步骤：A method for preparing a aldehyde-free high-strength electromagnetic shielding wood fiber composite material, comprising the following steps:
(1)木质纤维改性处理：将木质纤维先分散到膨润土分散液中，然后调节分散液pH至10.0，添加马来酸酐，温度调节至80℃，保温搅拌1小时，调节分散液pH至中性，然后再进行旋转蒸发干燥，得到改性木质纤维；(1) Wood fiber modification treatment: first disperse the wood fiber into the bentonite dispersion, then adjust the pH of the dispersion to 10.0, add maleic anhydride, adjust the temperature to 80°C, keep stirring for 1 hour, and adjust the pH of the dispersion to medium property, and then carry out rotary evaporation drying to obtain modified wood fiber;
(2)配置聚乙烯醇溶液，将聚乙烯醇溶液添加到去离子水中，搅拌均匀，得到聚乙烯醇溶液；(2) configure polyvinyl alcohol solution, add polyvinyl alcohol solution to deionized water, stir evenly, obtain polyvinyl alcohol solution;
(3)将改性木质纤维与聚乙烯醇溶液混合到一起，搅拌均匀后，至于温度50℃下静置30min，得到中间料；(3) Mix the modified wood fiber and the polyvinyl alcohol solution together, after stirring evenly, let stand at a temperature of 50° C. for 30 minutes to obtain an intermediate material;
(4)将中间料、改性胶黏剂混合均匀后，进行铺装、热压、冷却，得到木质纤维复合材料。(4) After mixing the intermediate material and the modified adhesive evenly, paving, hot pressing, and cooling are carried out to obtain a wood fiber composite material.
所述木质纤维、膨润土分散液混合质量比为1:5；Described wood fiber, bentonite dispersion liquid mixing mass ratio are 1:5;
所述膨润土分散液质量分数为8％；The bentonite dispersion mass fraction is 8%;
所述膨润土分散液中膨润土粒度为100μm；The bentonite particle size in the bentonite dispersion is 100 μm;
所述木质纤维、马来酸酐质量比为10:1.5。The mass ratio of wood fiber to maleic anhydride is 10:1.5.
所述聚乙烯醇溶液质量分数为15％。The mass fraction of the polyvinyl alcohol solution is 15%.
所述改性木质纤维与聚乙烯醇溶液混合质量比为12:2。The mixing mass ratio of the modified wood fiber to the polyvinyl alcohol solution is 12:2.
所述改性胶黏剂按重量份计由以下成分制成：脲醛树脂500、纳米吸波剂5、羟甲基纤维素50、消泡剂5、纳米碳酸钙15、去离子水110。The modified adhesive is made of the following components in parts by weight: urea-formaldehyde resin 500, nano wave absorbing agent 5, hydroxymethyl cellulose 50, defoamer 5, nano calcium carbonate 15, deionized water 110.
所述的纳米核壳吸波剂制备方法：将Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑依次分散到甲醇中，磁力搅拌30min，然后进行，离心过滤，用乙醇清洗3次，放入真空干燥箱中，再添加到球磨机中进行球磨混合，混合1h；混合均匀后，再移入电阻炉中在1600℃，真空环境下煅烧4h，即得纳米核壳吸波剂；The preparation method of the nano-core-shell wave absorber: disperse Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene and 2-methylimidazole in methanol in sequence, stir magnetically for 30 minutes, and then conduct centrifugal filtration , washed with ethanol for 3 times, put into a vacuum drying oven, then added to a ball mill for ball milling and mixing, and mixed for 1 hour; after mixing evenly, then moved into a resistance furnace and calcined for 4 hours in a vacuum environment at 1600°C to obtain nano-core shells absorber;
所述真空干燥箱内真空干燥温度为50℃。The vacuum drying temperature in the vacuum drying oven is 50°C.
所述Co(NO3)2·6H2O、硅粉、石墨烯和2-甲基咪唑、甲醇混合重量份比为10:30:20:5:50。The mixing weight ratio of Co(NO 3 ) 2 ·6H 2 O, silicon powder, graphene, 2-methylimidazole and methanol is 10:30:20:5:50.
所述硅粉纯度为99.99％，粒度为1000目。The silicon powder has a purity of 99.99% and a particle size of 1000 mesh.
所述消泡剂为有机硅消泡剂。The defoamer is a silicone defoamer.
所述木质纤维复合材料中改性胶黏剂的施胶量为150kg/m3。The sizing amount of the modified adhesive in the wood fiber composite material is 150kg/m 3 .
试验test
电磁屏蔽性能Electromagnetic shielding performance
本试验采用立式法兰同轴测试仪对实施例与对比例试样进行电磁屏蔽效能测试，电磁波频率为1.2GHz：In this test, a vertical flange coaxial tester is used to test the electromagnetic shielding effectiveness of the examples and comparative samples, and the electromagnetic wave frequency is 1.2GHz:
表1Table 1
对比例1：与实施例1区别为纳米核壳吸波剂中不添加Co(NO3)2·6H2O；Comparative Example 1: The difference from Example 1 is that Co(NO 3 ) 2 ·6H 2 O is not added to the nano core-shell wave absorbing agent;
对比例2：与实施例1区别为不添加纳米核壳吸波剂；Comparative Example 2: The difference from Example 1 is that no nano core-shell wave absorbing agent is added;
由表1可以看出，本发明制备木质纤维复合材料具有优异的电磁屏蔽性能，本发明通过引入制备的纳米核壳吸波剂，能够大幅度的改善木质纤维复合材料的电磁屏蔽性能。It can be seen from Table 1 that the wood fiber composite material prepared by the present invention has excellent electromagnetic shielding performance, and the present invention can greatly improve the electromagnetic shielding performance of the wood fiber composite material by introducing the prepared nano core-shell absorber.
进一步实验，对实施例试样依照国家标准GB/T 39598-2021进行检测：For further experiments, the samples of the examples were tested according to the national standard GB/T 39598-2021:
表2Table 2
由表2可以看出，本发明制备的木质纤维板甲醛释放符合国家标准，绿色环保，应用本发明的木质纤维板对人体健康具有更好的保障。It can be seen from Table 2 that the formaldehyde emission of the wood fiber board prepared by the present invention meets the national standard, and is environmentally friendly, and the application of the wood fiber board of the present invention has better protection for human health.
进一步实验，根据国家标准GB/T 11718-1999对实施例与对比例试样性能，进行对比：Further experiment, according to national standard GB/T 11718-1999 to embodiment and comparative sample performance, compare:
表3table 3
对比例3：与实施例1区别为木质纤维不经过改性处理；Comparative Example 3: The difference from Example 1 is that the wood fiber is not modified;
对比例4：与实施例1区别为将改性胶黏剂替换为常规脲醛树脂胶黏剂；Comparative Example 4: The difference from Example 1 is that the modified adhesive is replaced by a conventional urea-formaldehyde resin adhesive;
由表3可以看出，本发明制备的木质纤维板的力学性能得到大幅度的提高，本发明通过对木质纤维的改性处理，能够改善了制备的木质纤维板的力学性能，同时配合改性胶黏剂的使用，进一步大幅度的增强了木质纤维板的力学性能。As can be seen from Table 3, the mechanical properties of the wood fiber board prepared by the present invention are greatly improved, and the present invention can improve the mechanical properties of the wood fiber board prepared by modifying the wood fiber. The use of additives further greatly enhanced the mechanical properties of wood fiberboard.
以实施例1为基础试样，对比不同纳米核壳吸波剂添加重量份对电磁屏蔽性能的影响。Taking Example 1 as the basic sample, the effects of different nano-core-shell absorbers by weight on the electromagnetic shielding performance were compared.
尽管已经示出和描述了本发明的实施例，对于本领域的普通技术人员而言，可以理解在不脱离本发明的原理和精神的情况下可以对这些实施例进行多种变化、修改、替换和变型，本发明的范围由所附权利要求及其等同物限定。Although the embodiments of the present invention have been shown and described, those skilled in the art can understand that various changes, modifications and substitutions can be made to these embodiments without departing from the principle and spirit of the present invention. and modifications, the scope of the invention is defined by the appended claims and their equivalents.
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