CN106573389B - 经处理的多孔材料 - Google Patents
经处理的多孔材料 Download PDFInfo
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Abstract
本发明描述一种经处理的纤维素材料,其包含:具有界定多个孔隙的多孔结构的纤维素材料,孔隙中的至少一部分含有处理剂,所述处理剂包含:包含烯烃‑羧酸共聚物的聚合物;包含二价、三价或四价金属离子的调节剂。
Description
背景技术
多孔材料(如纤维素材料)需加以保护以防止霉变、昆虫袭击、腐烂以及浸水,从而有助于保持纤维素材料的物理特性。这种纤维素材料的一个实例是木材。多种处理剂以及保藏方法已知可保藏纤维素材料。
现代保藏方法典型地涉及用处理剂压缩处理纤维素材料。压缩处理典型地让处理剂渗入纤维素材料的整个多孔结构中。处理剂典型地是一种为了赋予纤维素材料所要物理特性而选择的化合物。举例而言,提高纤维素材料硬度、增加纤维素材料耐水性以及改善纤维素材料尺寸稳定性的处理剂是令人感兴趣的。木材在水中的吸收能力多达其重量的100%,从而引起木材胀大,在经由蒸发而发生水损失之后,引起木材收缩。这个水吸收/蒸发过程是不均一的且在木材中产生内应力,导致裂开、翘曲、弓形、弯曲、扭曲、卷曲等。另外,水能够充当使纤维素材料降解的生物体(如昆虫或真菌)的路径。驱赶昆虫或使真菌/霉菌形成减到最少或改善纤维素材料整体耐久性的处理剂是令人感兴趣的。另外,处理剂能够改善抗风性、紫外辐射抗性、高温以及低温下的稳定性、抗害虫性、抗霉性、防火性以及可能影响纤维素材料物理特性的其它问题。
经改进的纤维素材料处理剂是所期望的。
发明内容
本发明描述一种经处理的纤维素材料,其包含:具有界定多个孔隙的多孔结构的纤维素材料,孔隙中的至少一部分含有处理剂,所述处理剂包含:包含烯烃-羧酸共聚物的聚合物;包含二价、三价或四价金属离子或其混合物的调节剂。
本发明更描述一种制备经处理的纤维素材料的方法,所述方法包括:(a)提供纤维素材料;(b)第一处理方案,所述第一处理方案包括用包含聚合物的水性分散液浸渍纤维素材料,所述聚合物包含烯烃-羧酸共聚物;及(c)第二处理方案,所述第二处理方案包括用调节剂浸渍纤维素材料,所述调节剂包含二价、三价或四价金属离子,或其混合物。
具体实施方式
如本文所用,术语“多孔材料”是指一种可渗透的材料,以便流体可借助于孔隙或其它通道而流经其中。多孔材料的一个实例是纤维素材料。多孔材料的其它实例包括石头、混凝土、陶瓷和其衍生物。如本文所用,术语“纤维素材料”是指一种包含纤维素作为结构组分的材料。纤维素材料的实例包括木材、纸、纺织品、绳索、颗粒板以及其它生物以及合成材料。如本文所用,木材包括实木以及所有木材复合材料(例如硬纸板、工程化木制品等)。纤维素材料一般具有界定多个孔隙的多孔结构。
“经处理的纤维素材料”是一种已经用处理剂处理以修改纤维素材料特性的纤维素材料。经处理剂修改的特性包括(但不限于)增强的疏水性、尺寸稳定性、抗真菌性、抗霉性、抗昆虫性、硬度、表面外观、UV稳定性、防火性以及可涂布性。通过降低水吸收和蒸发速率来增强纤维素材料的疏水性能够提供其它辅助益处,如尺寸稳定性,从而降低膨胀以及收缩的内应力。
“处理剂”是一种当与纤维素材料合并时修改纤维素材料特性的物质。在一个例子中,处理剂包含聚合物与调节剂。将处理剂施加到纤维素材料中。一种将处理剂施加到纤维素材料的方法是使用压缩处理进行浸渍。在一个例子中,聚合物是作为分散液的一部分施加到纤维素材料中。已知施加处理剂的其它方法,如刷涂、涂布、喷涂、浸涂、浸泡以及挤压。一旦施加,则处理剂将渗入纤维素材料的至少一部分孔隙中。
如本文所用,聚合物是指由一种或多种类型的单体形成的分子。聚合物优选共聚物或共聚物与聚合物的混合物。如本文所用,共聚物可以指交替共聚物、周期共聚物、统计共聚物、无规共聚物、嵌段共聚物、接枝共聚物,或如所知的其它共聚物。如本文所用,共聚物是指通过合并两个或更多个单体所形成的聚合物。共聚物实例包括二元共聚物、三元共聚物、四元共聚物以及其它更高次元共聚物。在一个例子中,聚合物包含烯烃-羧酸共聚物。在一个例子中,烯烃-羧酸共聚物包含呈聚合形式的单体,所述单体选自包含以下各物的群组:乙烯、丙烯、1-丁烯、3-甲基-1-丁烯、4-甲基-1-戊烯、3-甲基-1-戊烯、1-庚烯、1-己烯、1-辛烯、1-癸烯、1-十二碳烯、丁二烯、苯乙烯、(甲基)丙烯酸、顺丁烯二酸、顺丁烯二酸酐,或其混合物。在一个例子中,苯乙烯丙烯酸分散液是适合的,例如可购自陶氏化学公司(TheDow Chemical Company)的OrotanTM CA-2005。存在于混合物中的其它适合聚合物及/或共聚物包括弹性体、塑料以及纤维。
在某些实施例中,聚合物包含极性烯烃聚合物,其具有极性基团作为共聚单体或接枝单体。如本文所用,极性烯烃聚合物是含有一个或多个极性基团的烯烃(共)聚合物。在示范性实施例中,聚合物可以例如包含一种或多种极性聚烯烃,其具有极性基团作为共聚单体或接枝单体。极性基团的实例包括羧酸、羧酸酐、羧酸酯、羧酸盐以及羧酸酰胺。示范性极性聚烯烃包括(但不限于)乙烯/丙烯酸(EAA)以及乙烯/甲基丙烯酸(EMAA)共聚物,如可购自陶氏化学公司的以商标PRIMACORTM可获得的那些聚烯烃;可购自杜邦公司(E.I.DuPontde Nemours)的NUCRELTM;以及可购自埃克森美孚化学公司(ExxonMobil ChemicalCompany)的ESCORTM。示范性共聚物还包括乙烯/顺丁烯二酸酐共聚物,如可以商标AMPLIFYTM GR获自陶氏化学公司的那些共聚物。示范性共聚物更包括乙烯/顺丁烯二酸酐以及丙烯/顺丁烯二酸酐共聚物,如可以商标LICOCENETM获自科莱恩国际有限公司(ClariantInternational Ltd.)的那些共聚物。其它示范性基质聚合物包括(但不限于)乙烯/乙酸乙烯酯共聚物、乙烯/丙烯酸乙酯(EEA)共聚物、乙烯/甲基丙烯酸甲酯(EMMA)共聚物以及乙烯丙烯酸丁酯(EBA)共聚物。
也可以使用其它烯烃-羧酸共聚物作为聚合物。具有酯或酸酐官能团的共聚物可以转化成羧酸或也可以通过本领域技术人员已知的方法对官能性羧酸盐进行化学修饰来使聚合物发生衍生化。还可以修饰聚合物以形成其它官能团,如酯或酰胺等。本领域的普通技术人员将认识到,还可以使用多种其它适用聚合物。
在一个实施例中,基质聚合物可以例如包含选自由以下组成的群组的极性聚烯烃:乙烯/丙烯酸(EAA)共聚物、乙烯/甲基丙烯酸共聚物(EMAA),及其组合。在一个例子中,聚合物包含单独或与其它聚合物或共聚物混合的乙烯/(甲基)丙烯酸共聚物。
如本文所使用,在如丙烯酸酯的另一术语之前使用术语“(甲基)”是指丙烯酸酯与甲基丙烯酸酯。举例来说,术语“(甲基)丙烯酸酯”是指丙烯酸酯或甲基丙烯酸酯;术语“(甲基)丙烯酸类”是指丙烯酸类或甲基丙烯酸类;且术语“(甲基)丙烯酸”是指丙烯酸或甲基丙烯酸。
在一个例子中,聚合物是水性分散液的组成部分。在一个例子中,分散液是包含聚合物、水以及一种或多种有机溶剂的介质。以分散液中的所悬浮颗粒尺寸适于渗入纤维素材料孔隙以便遍布于纤维素材料中的方式来制备水性分散液。在一个例子中,分散液还包含一种或多种添加剂。在一个例子中,存在于水性分散液中的任何固体保持于稳定悬浮液中且可通过分散于纤维素材料孔隙中来输送。在一个例子中,分散液的固体含量是聚合物与调节剂的组合重量的1重量%至75重量%。在一个例子中,有机溶剂是氧化溶剂、烃溶剂、卤化溶剂或其组合。
聚合物的羧酸部分用中和剂至少部分地中和以形成稳定水性分散液。如本文所用,中和剂是其中与羧酸的反应可潜在地引起盐形成的任何材料。在一个例子中,中和剂选自碱金属的氢氧化物、氨或其有机衍生物(包括胺)。在一个例子中,中和剂是强碱或弱碱。举例来说,中和剂可以是氢氧化钠、氢氧化钾或氨或胺,如单乙醇胺(MEA)、三乙醇胺(TEA)、二乙基乙醇胺(DEEA)或二甲基氨基乙醇(DMEA)。获自BYK USA公司的AQUACERTM 8804是中和EAA分散液的一个实例。稳定分散液是适于渗入纤维素材料孔隙的分散液。中和剂中和聚合物羧酸基团的至少一部分。如本文所用,羧酸基团的中和是指使羧酸基团中的氢转移的任何反应。在一个例子中,聚合物中5摩尔%到100摩尔%的羧酸基团通过中和剂中和。在另一个例子中,10到80摩尔%的羧酸基团通过中和剂中和。在仍然另一个例子中,20摩尔%到70摩尔%的羧酸基团通过中和剂中和。
调节剂是一种当与聚合物合并时修改至少一部分聚合物的物质。在一个例子中,调节剂与聚合物的至少一部分发生交联。在一个例子中,不受理论限制,调节剂与聚合物的至少一部分发生相互作用,以便调节剂至少部分地阻止聚合物从纤维素材料中移出。在一个例子中,调节剂是二价、三价金属或四价金属离子,或其混合物,其能够在水中形成稳定分散液且能够与聚合物交联。适合二价金属离子的实例包括Ca2+、Zn2+、Mg2+、Ba2+、Fe2+、Cu2+、Sn2+、S2+以及Ni2+,或其混合物。适合三价金属离子的实例包括Fe3+、B3+、P3+、Al3+、Cu3+、La3+、Y3+以及Ga3+,或其混合物。适合四价金属离子的实例包括Si4+、S4+、Ti4+、Zr4+、Sn4+、Ce4+以及Hf4+,或其混合物。在一个例子中,调节剂存在于具有溶剂的溶液中。
将处理剂与纤维素材料合并。在一个例子中,处理剂是通过压缩处理引入纤维素材料中,如本文所述。在一个例子中,压缩处理是在大于环境压力下进行。在一个例子中,压缩处理是在小于环境压力下进行。在另一例子中,处理剂是通过所属领域中已知的其它技术引入纤维素材料中,例如刷涂、涂布、浸涂、浸泡、喷涂以及挤压。处理剂浸入纤维素材料中的至少一部分孔隙中,且由此增加了纤维素材料的重量。在一个例子中,聚合物使纤维素材料的重量增加了1%到80%(如将纤维素材料干燥之后所计算)。在一个例子中,处理剂-聚合物与调节剂的组合-使纤维素材料的重量增加了5%到大于100%(如将纤维素材料干燥之后所计算)。
在一个例子中,处理剂包含一种或多种添加剂。添加剂可以作为分散液的一部分、作为调节剂的一部分纳入,或可以与其分开纳入。已知使经处理的纤维素材料增添特性的添加剂是适合的,如阻燃剂、分散剂及/或染料。举例来说,添加剂可以是有机化合物、金属化合物或有机金属化合物。在一个例子中,添加剂是一种改善聚合物润湿于或渗透于木材中的材料,例如在分散液中稳定的溶剂或表面活性剂(阴离子、阳离子或非离子型)。添加剂实例包括溶剂、填充剂、增稠剂、乳化剂、分散剂、缓冲剂、颜料、渗透剂、抗静电剂、气味物质、腐蚀抑制剂、防腐剂、渗硅剂、流变改性剂、抗沉降剂、抗氧化剂、其它交联剂(例如二元醇以及多元醇)、光学增亮剂、蜡、聚结剂、杀生物剂以及消泡剂。这种蜡可以包括石油蜡、石蜡、天然蜡,或合成蜡,如聚乙烯蜡或氧化聚乙烯蜡、蜂蜡,或粗蜡。另外,处理剂可以结合木材防腐剂使用,所述木材防腐剂含有例如铜-氨、铜-胺、铜-氨-胺复合物、季铵化合物或其它系统。举例来说,处理剂可以结合碱性铜-季铵(Alkaline Copper-Quaternaryammonium;ACQ)防腐剂系统使用。处理剂还可以结合使用锌盐或含硼化合物的木材防腐技术使用。任选地,可以将其它添加剂(如杀虫剂、杀白蚁剂、杀真菌剂以及杀霉菌剂)加入处理剂中。在一个例子中,添加剂是作为分散液的一部分纳入且由此形成稳定悬浮液。在一个例子中,将一种或多种表面活性剂加入分散液中。在一个例子中,选择使聚合物在纤维素材料表面的胶凝减少的表面活性剂。在一个例子中,选择使浸入纤维素材料中的聚合物的量增加的表面活性剂。举例来说,适合的表面活性剂可以是非离子、阴离子或阳离子型。非离子型表面活性剂的实例包括:烷氧基化醇、烷氧基化烷基酚、脂肪酸酯、胺以及酰胺衍生物、烷基聚葡糖苷、环氧乙烷/环氧丙烷共聚物、多元醇以及烷氧基化多元醇。举例来说,非离子型表面活性剂是可购自陶氏化学公司的TERGITOLTM L-62。阴离子型表面活性剂的实例包括:烷基硫酸盐、烷基醚硫酸盐、硫酸化烷醇酰胺、α烯烃磺酸盐、木质素磺酸盐、磺基丁二酸盐、脂肪酸盐以及磷酸酯。举例来说,阴离子型表面活性剂是可购自陶氏化学公司的DOWFAXTM C10L。阳离子型表面活性剂的实例包括烷基三甲基铵盐。
在一个例子中,经处理的纤维素材料至少根据第一处理方案以及第二处理方案制备。在一个例子中,第一处理方案包含用聚合物浸渍纤维素材料。第一处理方案包含以下步骤中的一个或多个:(a)使根据第一处理方案所制备的纤维素材料在容器中沉积;(b)使容器在真空下保持5分钟到60分钟;(c)将分散液引入容器;(d)将容器加压到1.03MPa维持5分钟到60分钟;(e)排放过量分散液;(f)任选地通过真空来移出过量分散液;及(g)将纤维素材料在20℃到60℃下风干24小时到48小时。
在一个例子中,经处理的纤维素材料至少根据第一处理方案以及第二处理方案制备。在一个例子中,第一处理方案包含用聚合物浸渍纤维素材料。第一处理方案包含以下步骤中的一个或多个:(a)使纤维素材料在容器中沉积;(b)使容器在真空下保持5分钟到60分钟;(c)将聚合物引入容器中;(d)将容器加压到1.03MPa维持5分钟到60分钟;(e)排放过量聚合物;(f)任选地通过真空来移出过量聚合物;及(g)将纤维素材料在20℃到60℃下风干24小时到48小时。在一个例子中,聚合物是水性分散液的一部分。
若干个干燥步骤可以在一系列温度下进行,其中风干步骤的持续时间与温度成比例。适合的风干温度是在室温(约20℃)与180℃之间。干燥可以是在空气中、在氮气中或其它适合氛围中进行。
利用水浸测试,根据美国木材保护协会标准E4-11程序(经压缩处理的木材的拒水性标准测试方法)测定经处理的纤维素材料的拒水性。水浸测试包括:首先,提供包含如本文所述制备的经处理纤维素材料的经处理薄片,与包含根据本文所述第一处理方案处理(但其中分散液用蒸馏水替换)的纤维素材料的对照薄片;第二,测量经处理薄片与对照薄片的切向尺寸,以得到初始切向尺寸(T1)(其中切向尺寸垂直于纤维素材料的颗粒方向);第三,将经处理的薄片与对照薄片均放入维持在65±3%相对湿度以及21±3℃的调节室中,直至达成恒重;第四,将经处理的薄片与对照薄片均在24±3℃的蒸馏水中浸没30分钟;及第四,从水中移出后,测量经处理的薄片与对照薄片的切向尺寸,以得到后切向尺寸(T2)。
DoN是指聚合物中的羧酸官能团的中和度。
各个别薄片(经处理的薄片与对照薄片)的膨胀百分比(S)如下计算:
在本文的每个实例中,对照薄片的膨胀百分比是4.7%。
拒水效率(Water-repellency efficiency;WRE)用于确定处理剂向经处理的纤维素材料增添拒水特性的有效性。WRE如下计算:
S1是指未处理薄片的膨胀百分比;S2是指经处理薄片的膨胀百分比。根据E4-11,对于大部分户外应用来说,优选75%的最小WRE。未经任何处理的原始木材的WRE是0%。
经处理的纤维素材料的硬度是根据肖氏(硬度计)测试,使用D型硬度计(30°锥体,1.40mm直径,2.54mm延长,44.48N弹簧力)测定。硬度是使用D型硬度计,通过将纤维素材料放置于硬平坦表面上来测定,且硬度计的压脚是利用针对纤维素材料的指定弹簧力按压。在与纤维素材料接触的一秒内,记录硬度计上的量表的硬度值。每个纤维素材料样品进行至少五次硬度测试。本文中报导的硬度值是针对所指定纤维素材料进行的测试平均值。未处理薄片的硬度值是40。
以下实例说明本发明的某些方面,但本发明的范围不限于以下实例。
以下实例中的分散液是通过将聚合物与指定量的碱合并于120℃的加压混合容器中来制得,如所属领域中已知(例如适合分散液可以根据陶氏化学公司的“PRIMACOR共聚物的水性分散液的制备”来制备)。实例中的所有真空操作是在-0.00399MPa到-0.00267Mpa的范围内。
实例1
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器(Parr reactor)的底部。反应器压力设定为真空维持30分钟。将包含38重量%PRIMACORTM5980i(35%DoN(使用NH3),8.35pH,粒度113nm,38%固体浓度)和62重量%水的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为真空维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.86%;第一块薄片的WRE是81.7%。经处理的薄片的硬度使用D型硬度计测量为58.2。
实例2
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含20重量%PRIMACORTM5980(50%DoN(使用MEA),8.21pH,粒度117nm,19%固体浓度)和80重量%水的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为真空维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.49%;经处理的薄片的WRE是89.5%。经处理的薄片的硬度使用D型硬度计测量为57.2。
实例3
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含20重量%PRIMACORTM5990(100%DoN(使用DMEA),9.52pH,20%固体浓度)和80重量%水的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%FeCl3(水溶液)。反应器压力设定为真空维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.46%;经处理的薄片的WRE是90.27%。经处理的薄片的硬度使用D型硬度计测量为39.3。
实例4
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含10重量%PRIMACORTM5990i(60%DoN(使用MEA))、6wt%TERGITOLTM L-62和84%水的80ml分散液引入反应器中。TERGITOLTM L-62是用于增强聚合物渗透的非离子型表面活性剂。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。木材在处理之后的重量增加是30%。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是4.5%;经处理的薄片的WRE是3.5%。经处理的薄片的硬度使用D型硬度计测量为45.2。
实例5
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含10重量%PRIMACORTM5990i(60%DoN(使用MEA))和90重量%水的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。木材在处理之后的重量增加是19%。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是4.2%;经处理的薄片的WRE是10.1%。经处理的薄片的硬度使用D型硬度计测量为45。
实例6
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含94%PRIMACORTM5980i水性分散液(100%DoN(使用TEA),7.8pH,粒度13nm,20%固体浓度)和6%DOWFAXTM C10L表面活性剂的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为150psi维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.63%;第一块薄片的WRE是86.5%。经处理的薄片的硬度使用D型硬度计测量为55.4。
实例7
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含94重量%PRIMACORTM5980i水性分散液(105%DoN(使用NH3),9.16pH,粒度113nm,19.37%固体浓度)和6重量%C10L表面活性剂的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为150psi维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是1.45%;第一块薄片的WRE是69.1%。经处理的薄片的硬度使用D型硬度计测量为54.3。
比较实例8
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含94重量%PRIMACORTM5980i水性分散液(105%DoN(使用NH3),9.16pH,粒度113nm,19.37%固体浓度)和6重量%C10L表面活性剂的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%NaCl(水溶液)。反应器压力设定为150psi维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是4.2%;第一块薄片的WRE是11.04%。经处理的薄片的硬度使用D型硬度计测量为52.3。
实例9
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含94%PRIMACORTM5980i水性分散液(100%DoN(使用KOH),12.3pH,粒度6.6nm,22.8%固体浓度)和6%C10L表面活性剂的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为150psi维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.7%;第一块薄片的WRE是84.8%。经处理的薄片的硬度使用D型硬度计测量为52.1。
实例10
松木薄片(南方黄松,4cm×2cm×0.5cm)通过砝码(在此使用环)固持于帕尔反应器的底部。反应器压力设定为真空维持30分钟。将包含94重量%PRIMACORTM5980i水性分散液(105%DoN(使用NH3),9.16pH,粒度113nm,19.37%固体浓度)和6重量%C10L表面活性剂的80ml分散液引入反应器中。接着将反应器压力设定为1.03MPa,在氮气下维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时。薄片通过砝码而固持于反应器底部。向反应器中装填足以浸没薄片的40wt%CaCl2(水溶液)。反应器压力设定为200psi维持60分钟。接着将薄片放入烘箱中且在60℃风干48小时,由此得到经处理的薄片。经处理的薄片以及对照薄片各自根据E4-11程序处理。经处理的薄片的膨胀百分比是0.078%;第一块薄片的WRE是98.3%。经处理的薄片的硬度使用D型硬度计测量为51.3。
实例说明,当纤维素材料含有处理剂(包含聚合物与调节剂)时,获得的WRE结果有利。然而,在纤维素材料尚未用聚合物与调节剂处理的情况下,如比较实例4以及比较实例5以及比较实例8中,未获得有利的WRE结果。
Claims (3)
1.一种制备经处理的纤维素材料的方法,所述方法包括:
(a)提供纤维素材料,所述纤维素材料包含木材或木材复合材料;
(b)第一处理方案,包括用包含聚合物的水性分散液浸渍所述纤维素材料,所述聚合物包含烯烃-羧酸共聚物;以及然后
(c)第二处理方案,包括用调节剂浸渍所述纤维素材料,所述调节剂包含Ca2+、Zn2+、Mg2 +、Ba2+、Fe2+、Cu2+、Sn2+、S2+、Ni2+、Fe3+、B3+、P3+、Al3+、Cu3+、La3+、Y3+、Ga3+、Si4+、S4+、Ti4+、Zr4+、Sn4 +、Ce4+、Hf4+或其混合物。
2.根据权利要求1所述的方法,其中所述第一处理方案中的所述浸渍是在大于或低于环境的压力下进行。
3.根据权利要求1或2所述的方法,其中所述聚合物是乙烯/丙烯酸共聚物。
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