CN106660225A - 经处理的多孔材料 - Google Patents

经处理的多孔材料 Download PDF

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Publication number
CN106660225A
CN106660225A CN201580036629.4A CN201580036629A CN106660225A CN 106660225 A CN106660225 A CN 106660225A CN 201580036629 A CN201580036629 A CN 201580036629A CN 106660225 A CN106660225 A CN 106660225A
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CN
China
Prior art keywords
cellulosic material
amine
jing
processed
polymer
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Pending
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CN201580036629.4A
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English (en)
Inventor
陈雪
S·W·金
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Dow Global Technologies LLC
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Dow Global Technologies LLC
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Publication of CN106660225A publication Critical patent/CN106660225A/zh
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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
    • B27K3/34—Organic impregnating agents
    • B27K3/50—Mixtures of different organic impregnating agents
    • 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
    • B27K3/02—Processes; Apparatus
    • B27K3/0278—Processes; Apparatus involving an additional treatment during or after impregnation
    • B27K3/0292—Processes; Apparatus involving an additional treatment during or after impregnation for improving fixation
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    • A01N27/00—Biocides, pest repellants or attractants, or plant growth regulators containing hydrocarbons
    • A—HUMAN NECESSITIES
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    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02—Amines; Quaternary ammonium compounds
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    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
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    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
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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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    • B27K3/08—Impregnating by pressure, e.g. vacuum impregnation
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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
    • B27K3/15—Impregnating involving polymerisation including use of polymer-containing impregnating agents
    • B27K3/153—Without in-situ polymerisation, condensation, or cross-linking reactions
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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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    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B27K3/36—Aliphatic compounds
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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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    • B27K3/38—Aromatic compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
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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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    • B27K5/00—Treating of wood not provided for in groups B27K1/00, B27K3/00
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    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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    • C08L23/14—Copolymers of propene
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    • D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
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Abstract

本发明描述了一种经处理的纤维素材料，其包含：纤维素材料，其具有限定多个孔的多孔结构，所述孔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；以及包含疏水胺的改性剂。

Description

经处理的多孔材料
背景技术
多孔材料，例如纤维素材料需要防止霉菌生长、昆虫侵食、腐烂和水浸渍，从而有利于保持纤维素材料的物理性质。此类纤维素材料的一个实例是木材。已知保存纤维素材料的各种处理剂和保存方法。
现代保存方法典型地包括用处理剂对纤维素材料进行压力处理。压力处理典型地允许处理剂渗透纤维素材料的整个多孔结构。处理剂典型地是为赋予纤维素材料所需物理性质而选择的化学化合物。例如，提高硬度、增加耐水性和改善纤维素材料的空间稳定性的处理剂是令人感兴趣的。木材能够在水中吸收多达其重量的100％，这导致木材膨胀，之后通过蒸发损失水导致木材收缩。这种吸水/蒸发的过程是不均匀的，并且在木材中产生内部应力，导致***、翘曲、弓弯、弯曲、扭曲、杯突等。另外，水可以用作降解纤维素材料的微生物例如昆虫或真菌的通道。驱除昆虫或最小化真菌/霉菌形成或改善纤维素材料的整体耐久性的处理剂是令人感兴趣的。此外，处理剂可以改善风阻、耐紫外辐射性、高温和低温稳定性、抗虫性、抗霉性、耐火性和可能影响纤维素材料的物理性质的其它问题。
需要一种改善的纤维素材料处理剂。
发明内容
本发明描述了经处理的纤维素材料，其包含：纤维素材料，其具有限定多个孔的多孔结构，孔的至少一部分含有处理剂，处理剂包含：包含烯烃-羧酸共聚物的聚合物；和包含疏水胺的改性剂。
本发明进一步描述了制备经处理的纤维素材料的方法，所述方法包含：(a)提供纤维素材料；(b)第一处理方案，其包含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(c)第二处理方案，其包含用改性剂浸渍所述纤维素材料，所述改性剂包含疏水胺。
具体实施方式
如本文所用，术语“多孔材料”是指可渗透使得流体可通过孔或其它通道而移动通过的材料。多孔材料的实例是纤维素材料。多孔材料的其它实例包括石材、混凝土、陶瓷及其衍生物。如本文所用，术语“纤维素材料”是指包括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、纺织物、绳、刨花板以及其它生物和合成材料。如本文所用，木材包括实木和所有木材复合材料(例如，粗纸板、工程木制品等)。纤维素材料通常具有限定多个孔的多孔结构。
如本文所用，除非另有说明，否则短语“分子量”是指标称分子量。
“经处理的纤维素材料”是已经用处理剂处理以改变纤维素材料的性质的纤维素材料。通过处理剂改性的性质包括但不限于提高的疏水性、空间稳定性、耐真菌性、耐霉性、抗虫性、硬度、表面外观、UV稳定性、耐火性和可涂布性。提高纤维素材料的疏水性可通过降低水吸收和蒸发的速率，从而减小膨胀和收缩的内应力，提供其它辅助益处，例如空间稳定性。
“处理剂”是当与纤维素材料组合时改变纤维素材料的性质的物质。在一种情况中，处理剂包含聚合物和改性剂。将处理剂施加到纤维素材料上。将处理剂施加到纤维素材料的一种方法是通过使用压力处理的浸渍。在一种情况中，将聚合物作为分散液的一部分施加到纤维素材料上。施加处理剂的其它方法是已知的，例如刷涂、涂布、喷涂、浸渍、浸泡和挤出。一旦施加，处理剂将渗透纤维素材料的孔的至少一部分。
如本文所用，聚合物是指由一或多种类型的单体形成的分子。聚合物优选是共聚物或共聚物和聚合物的混合物。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、接枝共聚物或其它已知的共聚物。如本文所用，共聚物是指通过将两种或更多种单体联合形成的聚合物。共聚物的实例包括二元共聚物、三元共聚物、四元共聚物和其它更高级的共聚物。在一种情况中，聚合物包含烯烃-羧酸共聚物。在一种情况中，烯烃-羧酸共聚物包含单体，所述单体选自由以下组成的群组：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-己烯、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、马来酸、马来酸酐或其混合物。在一种情况中，苯乙烯丙烯酸分散液是合适的，例如可从陶氏化学公司(The Dow Chemical Company)商购的OrotanTM CA-2005。存在于混合物中的其它合适的聚合物和/或共聚物包括弹性体、塑料和纤维。
在某些实施例中，聚合物包含极性烯烃聚合物，其具有作为共聚单体或接枝单体的极性基团。如本文所用，极性烯烃聚合物是含有一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或多种极性聚烯烃，其具有作为共聚单体或接枝单体的极性基团。极性基团的实例包括羧酸、羧酸酐、羧酸酯、羧酸盐和羧酸酰胺。示范性极性聚烯烃包括但不限于乙烯/丙烯酸(EAA)和乙烯/甲基丙烯酸(EMAA)共聚物，例如可以商品名PRIMACORTM从陶氏化学公司商购可得的那些，从杜邦公司(EI DuPont de Nemours)商购可得的NUCRELTM，和从埃克森美孚化工公司(ExxonMobil Chemical Company)商购可得ESCORTM。示范性共聚物还包括乙烯/马来酸酐共聚物，例如可从陶氏化学公司以商标AMPLIFYTM GR获得的那些。示范性共聚物进一步包括乙烯/马来酸酐和丙烯/马来酸酐共聚物，例如以商标LICOCENETM得自科莱恩国际有限公司(Clariant International Ltd)的那些。其它示范性的基础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)共聚物和乙烯丙烯酸丁酯(EBA)共聚物。
其它烯烃-羧酸共聚物也可以用作聚合物。具有酯或酸酐官能团的共聚物可以转化成羧酸，或者也可以通过本领域技术人员已知的方法通过官能羧酸盐的化学改性得到聚合物。聚合物也可以被改性以形成其它官能团，例如酯或酰胺等。本领域普通技术人员将认识到也可以使用许多其它有用的聚合物。
在一个实施例中，基础聚合物可以例如包含极性聚烯烃，所述极性聚烯烃选自由以下组成的群组：乙烯/丙烯酸(EAA)共聚物、乙烯/甲基丙烯酸共聚物(EMAA)及其组合。在一种情况中，聚合物包含单独的乙烯/(甲基)丙烯酸共聚物，或与其它聚合物或共聚物的混合物。
如本文所用，术语“(甲基)”随后是另一术语如丙烯酸酯的使用是指丙烯酸酯和甲基丙烯酸酯。例如，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；术语“(甲基)丙烯酸”是指丙烯酸或甲基丙烯酸。
在一种情况中，聚合物是水性分散液的组成部分。在一种情况中，分散液是包含聚合物、水和一或多种有机溶剂的介质。制备水性分散液使得分散液中的悬浮粒径适于渗透纤维素材料的孔以分布贯通纤维素材料。在一种情况中，分散液还包含一或多种添加剂。在一种情况中，存在于水性分散液中的任何固体保持在稳定的悬浮液中，并且可通过分散液输送到纤维素材料的孔中。在一种情况中，分散液的固体含量为1到75重量百分比。在一种情况中，有机溶剂是氧化溶剂、烃溶剂、卤化溶剂或其组合。
用中和剂至少部分地中和聚合物的羧酸部分以形成稳定的水分散液。如本文所用，中和剂是其中与羧酸的反应可能导致盐形成的任何物质。在一种情况中，中和剂选自碱金属氢氧化物、氨或其有机衍生物(包括胺)。在一种情况中，中和剂是强碱或弱碱。例如，中和剂可以是氢氧化钠、氢氧化钾或氨或胺，例如单乙醇胺(MEA)、三乙醇胺(TEA)、二乙基乙醇胺(DEEA)或二甲基氨基乙醇(DMEA)。得自BYK美国公司(BYK USA Inc)的AQUACERTM 8804是中和的EAA分散液的实例。稳定的分散液是适于渗透纤维素材料的孔的分散液。中和剂中和聚合物的羧酸基团的至少一部分。如本文所用，羧酸基团的中和是指其中羧酸基团的氢被转移的任何反应。在一种情况中，聚合物的5到100摩尔百分比的羧酸基团被中和剂中和。在另一种情况中，10到80摩尔百分比的羧酸基团被中和剂中和。在另一个实例中，20到70摩尔百分比的羧酸基团被中和剂中和。
改性剂是当与聚合物组合时改变聚合物的羧酸基团的至少一部分的物质。在一种情况中，改性剂是疏水胺，例如伯胺、仲胺或叔胺。在一种情况中，改性剂是疏水胺盐。在一种情况中，疏水胺仅含有一个氨基。疏水胺可以是任何合适的胺，例如直链胺、支链脂族胺、环胺、芳族胺或其混合物。选择胺使得粘度足够低以渗透纤维素材料的孔并且包含六个或更多个碳原子以提供足够的疏水性。在高粘度胺或固体胺的情况下，可以使用溶剂，例如水、氧化溶剂、卤化溶剂、芳族溶剂或烃。疏水胺的实例包括N-甲基N-己胺、N，N-二乙基正己胺、正辛胺、正癸胺正十二烷胺、N-甲基环己胺、N，N，-二乙基环己胺、二环己胺、苄胺、椰油胺、油胺、硬脂胺和N，N-二甲基取代的脂肪胺。在一个实例中，改性剂是苯乙胺或牛脂胺。在一个实例中，改性剂是聚醚胺(例如，购自亨斯迈公司(Huntsman Company)的M-2005或 M-600)。
处理剂与纤维素材料组合。在一种情况中，如本文所述，通过压力处理将处理剂引入纤维素材料。在另一种情况中，通过本领域已知的其它技术，例如刷涂、涂布、浸渍、浸泡、喷涂和挤出将处理剂引入纤维素材料。处理剂变得浸渍在纤维素材料的孔的至少一部分中，从而增加纤维素材料的重量。在一种情况中，聚合物将纤维素材料的重量增加1到80百分比(在干燥纤维素材料之后计算)。在一种情况中，处理剂(聚合物和改性剂的组合)将纤维素材料的重量增加5到大于100百分比(在干燥纤维素材料后计算)。
在一种情况中，处理剂包含一或多种添加剂。添加剂可以作为分散液的一部分包含，作为改性剂的一部分，或者可以与其分开包括。为处理的纤维素材料增加性质的已知添加剂是合适的，例如阻燃剂、分散剂和/或染料。例如，添加剂可以是有机化合物、金属化合物或有机金属化合物。在一种情况中，添加剂是改善聚合物润湿或渗透到木材中的材料，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)。添加剂的实例包括溶剂、填料、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(例如二醇和多元醇)、光学增白剂、蜡、聚结剂、杀生物剂和消泡剂。此类蜡可以包括石油蜡、石蜡、天然蜡或合成蜡如聚乙烯蜡或氧化聚乙烯蜡、蜂蜡或疏松蜡。此外，处理剂可以与含有例如铜氨、铜胺、铜氨-胺络合物、季铵化合物或其他体系的木材防腐剂结合使用。例如，处理剂可以与碱性铜-季铵(ACQ)防腐剂体系一起使用。处理剂也可以与使用锌盐或含硼化合物的木材防腐技术一起使用。任选地，可以向处理剂中加入其它添加剂，例如杀虫剂、杀白蚁剂、杀真菌剂和杀霉菌剂。在一种情况中，添加剂作为分散液的一部分被包括并与其形成稳定的悬浮液。在一种情况中，将一或多种表面活性剂加入到分散液中。在一种情况中，选择降低聚合物在纤维素材料表面的胶凝的表面活性剂。在一种情况中，选择增加浸渍在纤维素材料中的聚合物的量的表面活性剂。例如，合适的表面活性剂可以是非离子、阴离子或阳离子的。非离子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、胺和酰胺衍生物、烷基聚葡糖苷、环氧乙烷/环氧丙烷共聚物、多元醇和烷氧基化多元醇。例如，非离子表面活性剂是可从陶氏化学公司商购的TERGITOLTM L-62。阴离子表面活性剂的实例包括：烷基硫酸盐、烷基醚硫酸盐、硫酸化链烷醇酰胺、α-烯烃磺酸盐、木素磺酸盐、磺基琥珀酸盐、脂肪酸盐和磷酸酯。例如，阴离子表面活性剂是可从陶氏化学公司商购的DOWFAXTM C10L。阳离子表面活性剂的实例包括烷基三甲基铵盐。
在一种情况中，通过压力处理将纤维素材料制备为经处理的纤维素材料。用于压力处理纤维素材料的压力可以高于或低于大气压。在一种情况中，压力低于环境压力，例如，0.0001到0.09MPa(0.75到675mmHg)。在另一种情况中，压力高于环境压力，例如，0.1到1.7MPa(750到12750mmHg)。设想本领域已知的压力处理方法适合于用处理剂浸渍纤维素材料。
在一种情况中，通过压力处理将纤维素材料制备为经处理的纤维素材料。用于压力处理纤维素材料的压力可以高于或低于大气压。在一种情况中，压力低于环境压力，例如，0.0001到0.09MPa(0.75到675mmHg)。在另一种情况中，压力高于环境压力，例如，0.1到1.7MPa(750到12750mmHg)。设想本领域已知的压力处理方法适合于用处理剂浸渍纤维素材料。
在一种情况中，根据至少第一处理方案和第二处理方案制备经处理的纤维素材料。在一种情况中，第一处理方案包含用聚合物浸渍纤维素材料。第一处理方案包含一或多个以下步骤：(a)将纤维素材料沉积在容器中；(b)将容器在真空下保持5到60分钟；(c)将聚合物引入容器中；(d)将容器加压至1.03MPa持续5到60分钟；(e)排出过量的聚合物；(f)任选地通过真空除去过量的聚合物；以及(g)在20到60℃下将纤维素材料空气干燥24到48小时。在一种情况中，聚合物是水分散液的一部分。
在一种情况中，随后根据用改性剂浸渍纤维素材料的第二处理方案制备第一处理方案的产物。第二处理方案包含一或多个以下步骤：(a)将根据第一处理方案制备的纤维素材料沉积在容器中；(b)将改性剂引入容器中；(c)将容器在真空或升高的压力下保持5到60分钟；(d)任选地通过真空除去过量的改性剂；以及(e)在60℃下将纤维素材料空气干燥24到48小时。
在一种情况中，随后根据中和方案中和第二处理方案的产物，所述中和方案通过使用改性剂中和剂中和来自第二处理方案的任何残留的改性剂。在一种情况中，改性剂中和剂是适于与改性剂反应以降低其碱性的任何材料，例如分散液。中和方案包含一或多个以下步骤：(a)将根据第二处理方案制备的纤维素材料沉积在容器中；(b)将改性剂中和剂引入容器中30分钟；以及(c)在60℃下将纤维素材料空气干燥24到48小时。
几个干燥步骤可以在一定温度范围内进行，由此空气干燥步骤的持续时间与温度成比例。合适的空气干燥温度在室温(约20℃)和180℃之间。干燥可以在空气、氮气或其它合适的气氛中进行。
根据美国木材保护协会标准E4-11程序(测试压力处理木材的拒水性的标准方法)，使用水浸渍试验来测定经处理的纤维素材料的拒水性。水浸渍试验包括：一、提供包含如本文所述制备的经处理的纤维素材料的经处理的薄片和对照薄片，所述对照薄片包含除了所述分散液被蒸馏水替换外根据本文所述的第一处理方案处理的纤维素材料；二、测量经处理的薄片和对照薄片的切向度以提供初始切向度(T1)(其中切向度垂直于纤维素材料的颗粒的方向)；三、将处理过的薄片和对照薄片放置在保持在65±3％相对湿度和21±3℃的调节室中，直到达到恒重；四、将处理过的薄片和对照薄片浸入24±3℃的蒸馏水中30分钟；以及四、测量在从水中移除之后处理的薄片和对照薄片的切向度，以提供后切线度(T2)。
DoN是指聚合物中羧酸官能团的中和度。
每个单独薄片(经处理的薄片和对照薄片)的膨胀百分比(S)如下计算：
本文的每个实例中，对照薄片的膨胀百分比为4.7％。
防水效率(WRE)用于确定处理剂在向经处理的纤维素材料添加防水性方面的有效性。WRE如下计算：
S1是指未经处理的薄片的膨胀百分比；S2是指经处理的薄片的膨胀百分比。根据E4-11，对于大多数户外应用，优选最小wRE为75％。
根据使用D型硬度计(30°锥，1.40mm直径，2.54mm延伸，44.48N弹簧力)的肖氏(硬度计)试验测定经处理的纤维素材料的硬度。使用D型硬度计，通过将纤维素材料放置在硬的平坦表面上，并且用给定的弹簧力将硬度计的底部压在纤维素材料上来测定硬度。在与纤维素材料接触的一秒内，从硬度计上的计量器记录硬度值。对每个纤维素材料样品进行至少五次硬度测试。本文报道的硬度值是对给定纤维素材料进行的测试的平均值。经处理的薄片的硬度值为40。
以下实例说明了本发明的某些方面，但是本发明的范围不限于以下实例。
在下列实例中的分散液是如本领域已知的通过将聚合物与给定量的碱在120℃的混合、加压容器中混合而制备(例如，合适的分散液可以由陶氏化学公司根据“PRIMACOR共聚物的水性分散液的制备”制备)。实例中的所有真空操作在-0.00399MPa到-0.00267MPa的范围内。
实例1
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器(Parr reactor)的底部。将反应器压力设定为真空持续30分钟。将80ml包含20重量百分比的PRIMACORTM 5980i(50％DoN与MEA，8.21pH，粒径为117nm，19％固体浓度)和80重量百分比水的分散液引入反应器中。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的苯乙胺(PEA)填充反应器以浸没薄片。将反应器压力设定为真空持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。经处理的薄片和对照薄片各自根据E4-11程序进行处理。第一片薄片的膨胀百分比为0.27％；第一片薄片的WRE为94.1％。使用D型硬度计测量经处理的薄片的硬度为57.9。
实例2
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含20重量百分比的PRIMACORTM5980i(50％DoN与MEA，8.21pH，粒径为117nm，19％固体浓度)和80重量百分比水的分散液引入反应器中。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的牛脂胺(在2-丁氧基乙醇中30重量百分比的牛脂胺)填充反应器以浸没薄片。将反应器压力设定为真空持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。薄片和对照薄片各自根据E4-11程序进行处理。经处理的薄片的膨胀百分比为0.87％；经处理的薄片的WRE为80.9％。使用D型硬度计测量经处理的薄片的硬度为51.0。
实例3
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含20重量百分比PRIMACORTM 5980i(50％DoN与TEA，20％固体浓度)和80重量百分比水的分散液引入反应器中。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的苯乙胺(PEA)填充反应器以浸没薄片。将反应器压力设定为真空持续60分钟。然后将第一片薄片放置在烘箱中并在60℃下空气干燥48小时，从而提供经处理的薄片。经处理的薄片和对照薄片各自根据E4-11程序进行处理。经处理的薄片的膨胀百分比为0.95％；经处理的薄片的WRE为78.52％。使用D型硬度计测量经处理的薄片的硬度为55.2。
实例4
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含20重量百分比PRIMACORTM 5990(100％DoN与DMEA，9.52pH，20％固体浓度)和80重量百分比水的分散液引入反应器中。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的苯乙胺(PEA)填充反应器以浸没薄片。将反应器压力设定为真空持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。经处理的薄片和对照薄片各自根据E4-11程序进行处理。经处理的薄片的膨胀百分比为0.7％；经处理的薄片的WRE为85.03％。使用D型硬度计将处理的薄片的硬度测量为56.5。
实例5
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(在此使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含10重量百分比PRIMACORTM 5990i(60％DoN与MEA)，6重量百分比TERGITOLTM L-62和84％水的分散液引入反应器中。TERGITOLTM L-62是由陶氏化学公司制造的非离子表面活性剂。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。木材处理后的重量增加为30％。经处理的薄片和对照薄片各自根据E4-11程序进行处理。经处理的薄片的膨胀百分比为4.5％；经处理后的薄片的WRE为3.5％。使用D型硬度计测量经处理的薄片的硬度为45.2。
实例6
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含20重量百分比PRIMACORTM 5990i(60％DoN与MEA，10％固体浓度)和80重量百分比水的分散液引入反应器中。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。木材处理后的重量增加为19％。经处理的薄片和对照薄片各自根据E4-11程序进行处理。经处理的薄片的膨胀百分比为4.2％；经处理后的薄片的WRE为10.1％。使用D型硬度计将处理的薄片的硬度测量为45.0
实例7
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含94重量百分比PRIMACORTM 5980i水性分散液(60％DoN与TEA，7.8pH，粒径为18.5nm，24％固体浓度)和6重量百分比的DOWFAXTM C10L的分散液引入反应器。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的10重量百分比的 M-2005水溶液填充反应器以浸没薄片。购自亨斯迈公司的 M-2005聚醚胺是具有约29/6的PO/EO比的标称2000分子量的单胺。反应器压力设定为150psi持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。经处理的薄片和对照薄片各自根据E4-11程序进行处理。第一片薄片的膨胀百分比为0.8％；第一片薄片的WRE为82.7％。使用D型硬度计测量经处理的薄片的硬度为53.9。
实例8
松木片(南方黄松，4cm×2cm×0.5cm)通过重物(这里使用环)保持在帕尔反应器的底部。将反应器压力设定为真空持续30分钟。将80ml包含94重量百分比PRIMACORTM 5980i水性分散液(60％DoN与TEA，7.8pH，粒径为18.5nm，24％固体浓度)和6重量百分比的DOWFAXTM C10L的分散液引入反应器。然后在氮气下将反应器压力设定为1.03MPa持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时。薄片通过重物保持在反应器的底部。用足够的10重量百分比的 M-600水溶液填充反应器以浸没薄片。购自亨斯迈公司的 M-600聚醚胺是600分子量的聚丙二醇单胺，在另一端具有甲氧基乙基封端。反应器压力设定为150psi持续60分钟。然后将薄片放置在烘箱中并在60℃下空气干燥48小时，由此提供经处理的薄片。经处理的薄片和对照薄片各自根据E4-11程序进行处理。第一片薄片的膨胀百分比为2.2％；第一片薄片的WRE为52.8％。使用D型硬度计测量经处理的薄片的硬度为52.2。
实例说明当纤维素材料含有处理剂(包括聚合物和改性剂两者)时，获得了有利的WRE结果。然而，在纤维素材料没有被聚合物和改性剂两者处理，例如比较例5和6中时，则不能获得有利的WRE结果。

Claims (15)

1.一种经处理的纤维素材料，其包含：
纤维素材料，其具有限定多个孔的多孔结构，所述孔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；以及
包含疏水胺的改性剂。
2.根据权利要求1所述的经处理的纤维素材料，其中所述共聚物的羧酸基团的至少一部分被中和。
3.根据权利要求1-2中任一权利要求所述的经处理的纤维素材料，其中所述烯烃-羧酸共聚物以聚合形式包含单体，所述单体选自由以下组成的群组：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、苯乙烯或其混合物。
4.根据权利要求1-3中任一权利要求所述的经处理的纤维素材料，其中所述烯烃-羧酸共聚物以聚合形式包含羧酸单体或酸酐单体，所述羧酸单体或酸酐单体选自由以下组成的群组：(甲基)丙烯酸、马来酸、马来酸酸酐或其混合物。
5.根据权利要求1-4中任一权利要求所述的经处理的纤维素材料，其中除了所述烯烃-羧酸共聚物以外，所述聚合物还包含一或多种聚合物。
6.根据权利要求1-5中任一权利要求所述的经处理的纤维素材料，其中所述改性剂是含有六个或更多个碳原子的伯胺、仲胺或叔胺。
7.根据权利要求1-6中任一权利要求所述的经处理的纤维素材料，其中所述改性剂包含N-甲基N-己胺、N，N-二乙基正己胺、正辛胺、正癸胺正十二烷胺、N-甲基环己胺、N，N，-二乙基环己胺、二环己胺、苄胺、椰油胺、油胺、硬脂胺、N，N-二甲基取代的脂肪胺、苯乙胺或牛脂胺。
8.根据权利要求1-7中任一权利要求所述的经处理的纤维素材料，其中所述改性剂中和所述聚合物的至少一部分。
9.根据权利要求1-8中任一权利要求所述的经处理的纤维素材料，其中所述聚合物是乙烯-丙烯酸共聚物。
10.根据权利要求1-9中任一权利要求所述的经处理的纤维素材料，其中所述经处理的纤维素材料通过(1)用包含所述聚合物的水性分散液浸渍所述纤维素材料以及(2)用所述改性剂浸渍所述纤维素材料来制备。
11.根据权利要求1-10中任一权利要求所述的经处理的纤维素材料，其中所述处理剂进一步包含一种或多种添加剂。
12.一种用于制备经处理的纤维素材料的方法，所述方法包含：
(a)提供纤维素材料；
(b)第一处理方案，其包含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
(c)第二处理方案，其包含用改性剂浸渍所述纤维素材料，所述改性剂包含疏水胺。
13.根据权利要求12所述的方法，其中所述第一处理方案的浸渍在高于或低于环境压力下进行。
14.根据权利要求12-13中任一权利要求所述的方法，其中所述改性剂包含N-甲基N-己胺、N，N-二乙基正己胺、正辛胺、正癸胺正十二烷胺、N-甲基环己胺、N，N，-二乙基环己胺、二环己胺、苄胺、椰油胺、油胺、硬脂胺、N，N-二甲基取代的脂肪胺、苯乙胺或牛脂胺。
15.根据权利要求12-14中任一权利要求所述的方法，其中所述聚合物是乙烯-丙烯酸共聚物。
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AU2015284276B2 (en) 2019-01-31
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US20170274552A1 (en) 2017-09-28
US10059026B2 (en) 2018-08-28

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