CN110919804B - 一种竹木材增强增效处理方法 - Google Patents
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Abstract
本发明涉及一种竹木材增强增效处理方法。本发明采用硫酸水解法制备纳米纤维素分散液,以一定浓度的纳米纤维素分散液为前驱液,在纳米纤维素表面原位生成纳米氧化锌,并对纤维素分散液进行复配改良,采用特定的方式浸渍到竹木材孔隙中,起填充、粘结和增强木材组织的作用,使处理材的硬度强度、尺寸稳定增强,同时对防霉防腐性有明显的提高。本发明方法适合于速生材、人工林等材质比较疏松的木材增强增效处理,也适合于轻度腐朽材的增强修复。
Description
(一)技术领域
本发明涉及一种竹木材增强增效处理方法。
(二)背景技术
我国天然林资源匮乏,而人工林面积占世界第一。人工速生材到了成熟期,可以砍伐利用,但是速生材材质相对疏松,强度、硬度等不够,且防霉防腐性能较差。若能对速生材进行适当的材性改良,则能有效替代进口硬阔叶材,减少我国对进口材的依存度。
纳米纤维素(CNC)是从天然纤维中提取的一种纳米级纤维材料,具有高结晶度、高强度、较大的表面积、高反应活性和强吸附能力,纳米纤维素原料来源丰富,提取过程比较简单,具有生物降解性、环保性和生物相容性,其强度超过钢铁,被广泛应用于纸张、涂膜及合成材料增强处理。CNC的优异性能,如强吸附能力及生物相容性可用于木材的仿生固结剂。由于纳米材料的高比表面积和高反应活性,特别能够与木材组织或在木材孔隙内部相互作用。
纳米氧化锌在紫外光遮蔽、光催化和抗菌材料等方面表现出优越性。然而纳米粒子表面能大,直接沉积在木材表面或者细胞腔中容易发生团聚,若借助纳米纤维素将其均匀的分散后导入,可望解决这个难题。
(三)发明内容
本发明目的是提供一种竹木材增强增效处理方法。
本发明采用的技术方案是:
一种竹木材增强增效处理方法,所述方法包括:
(1)纳米纤维素分散液A制备:以脱脂棉或棉短绒为纤维来源,与浓度为60~70%的硫酸进行混合,硫酸溶液用量为10~40mL/g纤维;在40~60℃水浴反应30~40min后,加入8~10倍(蒸馏水体积为反应液体积8~10倍)蒸馏水终止反应,1200rpm离心15min,将沉淀物置于透析袋中在去离子水中透析至pH值恒定,使用孔径为0.22um的滤膜抽滤,稀释至终浓度为1~2%,即获得纳米纤维素分散液A;
(2)纳米氧化锌-纳米纤维素复合液B制备:以纳米纤维素分散液A作为纳米氧化锌的前驱体和保护液,加入ZnCl2水溶液,配制的纳米纤维素分散液A与ZnCl2混合液中ZnCl2浓度为0.1~1mmol/L,在60~80℃水浴中搅拌10~30min,生成的纳米ZnO晶体直接在纤维素基材上成核,获得纳米氧化锌-纳米纤维素复合液B;
(3)增强处理液配制:分别以质量浓度为0.8~1.0%的聚二甲基硅氧PDMS、质量浓度为1~1.5%的羟丙基纤维素HMC、质量浓度为0.5~1.0%的碱木质素Lignin和质量浓度为3~5%的酚醛树脂PF为处理液的增效剂,按下述体积比例与纳米纤维素分散液A(即CNC)进行复配,得到增强处理液a~e,具体如下:
a:CNC:PDMS=2:1混合,pH=8.4,常温磁力搅拌60min;
b:CNC:Lignin=2:1混合,pH=7.5,常温磁力搅拌60min;
c:CNC:PDMS:Lignin=2:1:1混合,pH=8.0,常温磁力搅拌60min;d:CNC:HMC=5:2混合,10000rpm高速搅拌混合;
e:CNC:PF=1:1混合,10000rpm高速搅拌混合。
(4)增强增效处理液1~5配制:步骤(4)增强处理液a~e与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8~1比例混合;
(5)竹木材增强、增效处理:样品用步骤(4)得到的增强增效处理液1~5浸渍处理,得到增强增效后的竹木材。
步骤(1)中硫酸用量优选为18~25mL/g纤维。
具体的,步骤(5)中所述浸渍可在真空度20mbar的真空釜中进行,浸渍时间3~6h,浸渍完成后103℃干燥至恒重,根据样品腐朽状况或预期目标情况,再继续浸渍,浸渍-干燥3~15个周期。
或者,步骤(5)中所述浸渍在100~200MPa压力下进行,浸渍时间30~60min,浸渍完成后再微波干燥。
又或者,步骤(5)中所述浸渍采用超高压浸渍-高温固化联合处理,浸渍压力100~200MPa,浸渍时间30~60min,浸渍完成后采用150~160℃高温进行固化。需要注意的是,采用增强增效处理液5时,必须使用超高压浸渍-高温固化联合处理的方法。
本发明采用硫酸水解法制备纳米纤维素分散液,以一定浓度的纳米纤维素分散液为前驱液和保护液,在纳米纤维素表面原位生成纳米氧化锌,并对纤维素分散液进行复配改良,采用特定的方式浸渍到竹木材孔隙中,起粘结和增强木材组织的作用,使处理材的硬度强度、尺寸稳定增强,同时对防霉、防腐性有明显的提高。本发明方法适合于速生材、人工林等材质比较疏松的木材增强增效处理,也适合于轻度腐朽材的增强修复。
本发明的有益效果主要体现在:采用本发明方法,竹木材经处理后硬度强度增强和尺寸稳定性增加,同时其防霉防腐性能也有明显的提高,非常适用于速生材、人工林等材质比较疏松的竹木材的增强增效处理,也适合于轻度腐朽材的增强修复。
(四)具体实施方式
下面结合具体实施例对本发明进行进一步描述,但本发明的保护范围并不仅限于此:
纳米纤维素分散液A制备:
以脱脂棉为纤维来源,与浓度为64%(w/w)的硫酸溶液进行混合,硫酸溶液用量为21mL/g纤维;在60℃水浴反应40min后,加入10倍蒸馏水终止反应,1200rpm离心15min,取沉淀物置于透析袋中在去离子水中透析至pH值恒定,然后使用孔径为0.22um的滤膜抽滤,稀释至终浓度为1.2%,即获得纳米纤维素分散液A。
纳米氧化锌-纳米纤维素复合液B制备:
以纳米纤维素分散液A作为纳米氧化锌的前驱体和保护液,加入浓度ZnCl2水溶液,纳米纤维素分散液A与ZnCl2混合液中ZnCl2的浓度为0.5mmol/L,在55℃水浴中搅拌20min,生成的纳米ZnO晶体直接在纤维素基材上成核,获得纳米氧化锌-纳米纤维素复合液B。
其他试剂配制:
CNC:浓度1%(w/w);
PDMS:浓度1%(w/w);
HMC:浓度1%(w/w);
Lignin:浓度1%(w/w);
PF:浓度5%(w/w)。
增强处理液a:CNC:PDMS=2:1混合(pH=8.4),常温磁力搅拌60min;
增强处理液b:CNC:Lignin=2:1混合(pH=7.5),常温磁力搅拌60min;
增强处理液c:CNC:Lignin:PDMS-NH=2:1:1混合(pH=8.0),常温磁力搅拌60min;
增强处理液d:CNC:HMC=5:2混合,10000rpm高速搅拌混合;
增强处理液e:CNC:PF=1:1混合,10000rpm高速搅拌混合;
增强增效处理液1:增强处理液a与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8比例混合;
增强增效处理液2:增强处理液b与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8比例混合;
增强增效处理液3:增强处理液c与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8比例混合;
增强增效处理液4:增强处理液d与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8比例混合;
增强增效处理液5:增强处理液e与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8比例混合。
实施例1:初腐马尾松增强处理
试材:初腐马尾松(50×50×20mm长×宽×厚)
将增强增效处理液1置于真空反应釜,将样品完全浸没,抽真空至20mbar,保持真空度3~6h,103℃干燥到恒重,再次浸渍,浸渍-干燥4个周期。再将增强增效处理液3如上步骤,浸渍-干燥3个周期。
初腐马尾松处理前后的性能测试结果见表1:
表1
由此可见,经处理后硬度及抗压强度增强,体积干缩率降低。
实施例2:毛竹材增效处理
试材:毛竹材(50×50×20mm长×宽×厚)
将增强、增效处理液2置于真空反应釜,将样品完全浸没,抽真空至20mbar,保持真空度3~6h,103℃干燥到恒重,再次浸渍,浸渍8个周期。
毛竹材处理前后的性能测试结果见表2:
表2
由此可见,经处理后体积干缩率降低,同时其防霉性能也有明显的提高。
实施例3:速生杨木增强增效处理
试材:杨木速生材(500×50×20mm长×宽×厚)
将增强增效处理液5置于厚塑料袋中,放入杨木速生材样品至浸没,抽真空塑封,然后置于超高压设备中,在100-200MPa条件下浸渍30min,103℃干燥到恒重,在100-200MPa条件下浸渍40min,取出后陈放1小时,置于150-160℃烘箱高温固化。
杨木速生材处理前后的性能测试结果见表3:
表3
由此可见,经处理后硬度和抗压强度增强,体积收缩率降低增加,同时防腐性能有明显的提高。
Claims (6)
1.一种竹木材增强增效处理方法,所述方法包括:
(1)纳米纤维素分散液A制备:以脱脂棉或棉短绒为纤维来源,与浓度为60~70%的硫酸进行混合,硫酸用量为10~40mL/g纤维;在40~60℃水浴反应30~40min后,加入8~10倍蒸馏水终止反应,1200rpm离心15min,将沉淀物置于透析袋中在去离子水中透析至pH值恒定,使用孔径为0.22um的滤膜抽滤,稀释至终浓度为1~2%,即获得纳米纤维素分散液A;
(2)纳米氧化锌-纳米纤维素复合液B制备:以纳米纤维素分散液作A为纳米氧化锌的前驱体和保护液,加入ZnCl2水溶液,配制的纳米纤维素分散液A与ZnCl2混合液中ZnCl2的浓度为0.1~1mmol/L,在60~80℃水浴中搅拌10~30min,生成的纳米ZnO晶体直接在纤维素基材上成核,获得纳米氧化锌-纳米纤维素复合液B;
(3)增强处理液配制:分别以质量浓度为0.8~1.0%的聚二甲基硅氧PDMS、质量浓度为1~1.5%的羟丙基纤维素HMC、质量浓度为0.5~1.0%的碱木质素Lignin和质量浓度为3~5%的酚醛树脂PF为处理液的粘合剂或增强剂,按下述体积比例与纳米纤维素分散液A进行复配,得到增强处理液a~e,具体如下:
a:CNC:PDMS=2:1混合,pH=8.4,常温磁力搅拌60min;
b:CNC:Lignin=2:1混合,pH=7.5,常温磁力搅拌60min;
c:CNC:PDMS:Lignin=2:1:1混合,pH=8.0,常温磁力搅拌60min;
d:CNC:HMC=5:2混合,10000rpm高速搅拌混合;
e:CNC:PF=1:1混合,10000rpm高速搅拌混合;
(4)增强增效处理液1~5配制:步骤(4)增强处理液a~e与纳米氧化锌-纳米纤维素复合液B按照体积比1:0.8~1.0比例混合,分别得到增强增效处理液1~5;
(5)竹木材增强、增效处理:样品用步骤(4)得到的增强增效处理液1~5进行浸渍处理,得到增强增效后的竹木材。
2.如权利要求1所述的方法,其特征在于步骤(1)中硫酸用量为18~25mL/g纤维。
3.如权利要求1所述的方法,其特征在于步骤(5)中所述浸渍在真空度20mbar的真空釜中进行,浸渍时间3~6h,浸渍完成后103℃干燥到恒重,根据样品腐朽状况或预期目标情况,再继续浸渍,浸渍-干燥周期3~15个周期。
4.如权利要求1所述的方法,其特征在于步骤(5)中所述浸渍在100~200MPa压力下进行,浸渍时间30~60min,浸渍完成后再微波干燥。
5.如权利要求1所述的方法,其特征在于步骤(5)中所述浸渍采用超高压浸渍-高温固化联合处理,浸渍压力100~200MPa,浸渍时间30~60min,浸渍完成后采用150~160℃高温进行固化。
6.如权利要求5所述的方法,其特征在于所用增强增效处理液为增强增效处理液5。
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