TW201439135A - 自由基聚合性樹脂組合物、底漆及地板防水結構體 - Google Patents
自由基聚合性樹脂組合物、底漆及地板防水結構體 Download PDFInfo
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- TW201439135A TW201439135A TW102145434A TW102145434A TW201439135A TW 201439135 A TW201439135 A TW 201439135A TW 102145434 A TW102145434 A TW 102145434A TW 102145434 A TW102145434 A TW 102145434A TW 201439135 A TW201439135 A TW 201439135A
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- C08F20/00—Homopolymers and copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride, ester, amide, imide or nitrile thereof
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- C08F290/00—Macromolecular compounds obtained by polymerising monomers on to polymers modified by introduction of aliphatic unsaturated end or side groups
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Abstract
本發明提供一種自由基聚合性樹脂組合物、以及使用其所獲得之底漆、地板防水結構體,上述自由基聚合性樹脂組合物之特徵在於:其含有自由基聚合性樹脂(A)、空氣乾燥性化合物(B)、自由基聚合性單體(C)及瀝青(D),且上述瀝青(D)之含量相對於上述樹脂(A)、上述化合物(B)及上述單體(C)之合計100質量份為0.01~25質量份之範圍。本發明之自由基聚合性樹脂組合物係防水層與瀝青鋪裝層之層間接著性優異之材料。又,其常溫乾燥性亦優異,並且亦可進行噴霧塗佈,因此,其亦可提高端部施工等之作業性。
Description
本發明係關於一種常溫乾燥性、及防水層與瀝青鋪裝層之層間接著性優異之自由基聚合性樹脂組合物、以及使用其所獲得之底漆及地板防水結構體。
近來,因增大之交通負荷或凍結防止劑之噴灑,以高速公路為代表之公路橋地板之早期劣化變得顯著。作為該早期劣化之機制,認為係通過產生於瀝青鋪裝與鋼筋混凝土地板間之裂紋,而使雨水、凍結防止劑等滲入至結構物中導致腐蝕鋼筋,使結構物之耐久性降低。
作為提高該等公路橋地板之耐久性之方法,業界對依序積層地板層、防水層、瀝青鋪裝層而構成之地板防水結構體進行各種研究。又,由於上述防水層與瀝青層間缺乏接著性,故而亦對用以提高層間接著性之方法進行各種研究。
作為上述方法,例如研究出於上述防水層與瀝青鋪裝層之層間插入多孔性熱塑性樹脂片之方法(例如參照專利文獻1)、或使用胺基甲酸酯系反應性熱熔接著劑之方法(例如參照專利文獻2)。
然而,該等之防水層與瀝青鋪裝層之層間接著性均不可謂充分,又,於插入多孔性熱塑性樹脂片之方法中,指出因使用片材而導致難以進行端部施工之缺點,或於使用胺基甲酸酯系反應性熱熔接著劑之方法中,指出因使用前必須在現場進行加溫等作業性較差之缺點。
因此,業界需求作業性良好且防水層與瀝青層之層間接著性優異之材料。
[專利文獻1]日本專利特開2005-113376號公報
[專利文獻2]日本專利特開2004-360325號公報
本發明所欲解決之問題在於提供一種常溫乾燥性、及防水層與瀝青鋪裝層之層間接著性優異之自由基聚合性樹脂組合物。
本發明者等在為解決上述問題而進行研究之過程中,為了提高防水層與瀝青鋪裝層之層間接著性而著眼於底漆之使用,進行努力研究。
結果發現,藉由於含有自由基聚合性樹脂、空氣乾燥性化合物及自由基聚合性單體之自由基聚合性樹脂組合物中進而含有特定量之瀝青,而可解決上述問題,從而完成本發明。
即,本發明提供一種自由基聚合性樹脂組合物、以及使用其所獲得之底漆、地板防水結構體,上述自由基聚合性樹脂組合物之特徵在於:其含有自由基聚合性樹脂(A)、空氣乾燥性化合物(B)、自由基聚合性單體(C)及瀝青(D),且上述瀝青(D)之含量相對於上述樹脂(A)、上述化合物(B)及上述單體(C)之合計100質量份為0.01~25質量份之範圍。
本發明之自由基聚合性樹脂組合物係防水層與瀝青鋪裝層之層間接著性優異者。又,其常溫乾燥性亦優異,並且亦可進行噴霧塗
佈,因此,其亦可提高端部施工等之作業性。
本發明之自由基聚合性樹脂組合物係含有自由基聚合性樹脂(A)、空氣乾燥性化合物(B)、自由基聚合性單體(C)及瀝青(D)者。
作為上述自由基聚合性樹脂(A),例如可列舉選自由不飽和聚酯、環氧(甲基)丙烯酸酯、(甲基)丙烯酸胺基甲酸酯、聚酯(甲基)丙烯酸酯所組成之群中之1種以上之自由基聚合性樹脂。
作為上述不飽和聚酯樹脂,例如可列舉利用先前公知之方法使含有α,β-不飽和二元酸之二元酸與多元醇進行反應而獲得者。
作為上述α,β-不飽和二元酸,例如可列舉:順丁烯二酸、順丁烯二酸酐、反丁烯二酸、伊康酸、伊康酸酐等。
作為其他二元酸,可使用飽和二元酸,例如可列舉:鄰苯二甲酸、鄰苯二甲酸酐、鹵代鄰苯二甲酸酐、間苯二甲酸、對苯二甲酸、四氫鄰苯二甲酸、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸、六氫鄰苯二甲酸酐、六氫對苯二甲酸、六氫間苯二甲酸、琥珀酸、丙二酸、戊二酸、己二酸、癸二酸、1,12-十二烷二酸、2,6-萘二羧酸、2,7-萘二羧酸、2,3-萘二羧酸、2,3-萘二羧酸酐、4,4'-聯苯二羧酸、或該等之二烷基酯等。
作為上述多元醇,例如可列舉:乙二醇、二乙二醇、三乙二醇、聚乙二醇、丙二醇、二丙二醇、聚丙二醇、2-甲基-1,3-丙二醇、1,3-丁二醇、新戊二醇、氫化雙酚A、1,4-丁二醇、雙酚A與環氧丙烷或環氧乙烷之加成物、1,2,3,4-四羥基丁烷、甘油、三羥甲基丙烷、1,3-丙二醇、1,2-環己烷二醇、1,3-環己烷二醇、1,4-環己烷二醇、1,4-環己烷二甲醇、對二甲苯二醇、二環己基-4,4'-二醇、2,6-十氫萘二醇、
2,7-十氫萘二醇等。
作為上述環氧(甲基)丙烯酸酯,可列舉利用先前公知之方法使雙酚型環氧化合物單獨與不飽和一元酸、或者使將雙酚型環氧化合物與酚醛清漆型環氧化合物加以混合而成之環氧化合物與不飽和一元酸進行反應而獲得者。
作為上述雙酚型環氧化合物,例如可列舉:藉由表氯醇與雙酚A或雙酚F之反應所獲得之1分子中具有2個以上環氧基之縮水甘油醚型環氧化合物、使甲基表氯醇與雙酚A或雙酚F進行反應而獲得之二甲基縮水甘油醚型環氧化合物、使雙酚A之環氧烷加成物與表氯醇或甲基表氯醇進行反應而獲得之環氧化合物等。
作為上述酚醛清漆型環氧化合物,例如可列舉:使苯酚酚醛清漆或甲酚酚醛清漆與表氯醇或甲基表氯醇進行反應而獲得之環氧化合物等。
作為上述不飽和一元酸,例如可列舉:(甲基)丙烯酸、肉桂酸、丁烯酸、順丁烯二酸單甲酯、順丁烯二酸單丙酯、順丁烯二酸單丁酯、山梨酸、順丁烯二酸單(2-乙基己基)酯等。
作為上述(甲基)丙烯酸胺基甲酸酯,例如可列舉利用先前公知之方法使多元醇、聚異氰酸酯及具有羥基之(甲基)丙烯酸系化合物進行反應而獲得者。
作為上述多元醇,例如可列舉:丙烯酸系多元醇、己內酯多元醇、丁二烯多元醇、聚醚多元醇、聚碳酸酯多元醇、聚酯多元醇等。
作為上述聚異氰酸酯,可列舉分子中具有2個以上異氰酸酯基者,例如可列舉:苯二異氰酸酯、二苯基甲烷二異氰酸酯、甲苯二異氰酸酯、萘二異氰酸酯等芳香族二異氰酸酯;六亞甲基二異氰酸酯、離胺酸二異氰酸酯、環己烷二異氰酸酯、異佛爾酮二異氰酸酯、4,4'-二環己基甲烷二異氰酸酯、苯二甲基二異氰酸酯、四甲基苯二甲基二
異氰酸酯等脂肪族或脂環式二異氰酸酯;苯二甲基二異氰酸酯、甲苯二異氰酸酯、二苯基甲烷二異氰酸酯、苯二異氰酸酯、聚伸苯基聚亞甲基聚異氰酸酯、亞甲基二苯基二異氰酸酯之福馬林縮合物,4,4'-二苯基甲烷二異氰酸酯之碳二醯亞胺改性物等芳香族系聚異氰酸酯等。
作為上述具有羥基之(甲基)丙烯酸系化合物,例如可列舉:(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸3-羥基丁酯、(甲基)丙烯酸4-羥基丁酯等具有羥基之(甲基)丙烯酸烷基酯,或聚乙二醇單丙烯酸酯、聚丙二醇單丙烯酸酯等。
再者,於本發明中,所謂「(甲基)丙烯酸酯」,係指甲基丙烯酸酯與丙烯酸酯中之一者或兩者,所謂「(甲基)丙烯醯基」,係指甲基丙烯醯基與丙烯醯基中之一者或兩者,所謂「(甲基)丙烯酸」,係指甲基丙烯酸與丙烯酸中之一者或兩者,所謂「(甲基)丙烯酸系化合物」,係指丙烯酸系化合物與甲基丙烯酸系化合物中之一者或兩者。
作為上述聚酯(甲基)丙烯酸酯,較佳為使用1分子中具有2個以上(甲基)丙烯醯基之飽和聚酯或不飽和聚酯。上述飽和聚酯係使飽和二元酸與多元醇進行縮合反應所得者,又,上述所謂不飽和聚酯係使α,β-不飽和二元酸與多元醇進行縮合反應所得者,且均於末端具有(甲基)丙烯醯基。
上述飽和二元酸、α,β-不飽和二元酸及上述多元醇可使用與上述不飽和聚酯之合成所使用之成分相同者。
作為上述聚酯(甲基)丙烯酸酯之製造方法,較佳為對飽和聚酯或不飽和聚酯使用(甲基)丙烯酸之縮水甘油酯化合物之方法,尤佳為使用(甲基)丙烯酸縮水甘油酯之方法。
作為上述空氣乾燥性化合物(B),可使用先前公知者,且可利用藉由使用具有空氣乾燥性賦予基之化合物(b-1)作為原料所獲得者。作為上述空氣乾燥性化合物(B),例如可列舉利用先前公知之方法使上
述化合物(b-1)與選自由α,β-不飽和二元酸、多元醇、芳香族飽和二元酸及其酸酐所組成之群中之1種以上之化合物(b-2)進行加成反應或酯化反應而獲得者。
作為上述化合物(b-1),例如可列舉選自由包含環狀不飽和脂肪族多元酸及其衍生物之化合物、包含具有α位氫之烯丙醚基之化合物、利用多元醇與乾性油之酯交換反應所獲得之醇解化合物、及包含具有羥基之二環戊二烯基之化合物所組成之群中之1種以上之化合物。該等化合物可單獨使用,亦可併用2種以上。
可用作上述化合物(b-2)之α,β-不飽和二元酸及多元醇能夠使用與可用於上述不飽和聚酯之製造之α,β-不飽和二元酸及多元醇相同者。
作為上述芳香族飽和二元酸及其酸酐,例如可列舉:鄰苯二甲酸、鄰苯二甲酸酐、鹵化鄰苯二甲酸酐、間苯二甲酸、對苯二甲酸、四氫鄰苯二甲酸、四氫鄰苯二甲酸酐、六氫鄰苯二甲酸、六氫鄰苯二甲酸酐、六氫對苯二甲酸、六氫間苯二甲酸、2,6-萘二羧酸、2,7-萘二羧酸、2,3-萘二羧酸、2,3-萘二羧酸酐、4,4'-聯苯二羧酸、以及該等之二烷基酯等。
關於上述自由基聚合性樹脂(A)與上述空氣乾燥性化合物(B)之質量比率[(A)/(B)],就常溫乾燥性或拉伸物性等方面而言,較佳為98/2~60/40之範圍,更佳為95/5~70/30之範圍,進而較佳為95/5~80/20之範圍。
上述自由基聚合性單體(C)係上述自由基聚合性樹脂(A)之反應性稀釋劑,例如可列舉:(甲基)丙烯酸甲酯、(甲基)丙烯酸乙酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸異丁酯、(甲基)丙烯酸第三丁酯、(甲基)丙烯酸己酯、(甲基)丙烯酸2-乙基己酯、(甲基)丙烯酸正辛酯、(甲基)丙烯酸癸酯、(甲基)丙烯酸2-羥基乙酯、(甲基)丙烯酸2-羥基丙酯、(甲基)丙烯酸β-乙氧基乙酯、(甲基)丙烯酸2-氰基乙酯、(甲基)丙
烯酸環己酯、(甲基)丙烯酸二乙基胺基乙酯、(甲基)丙烯酸月桂酯、(甲基)丙烯酸硬脂酯、聚己內酯(甲基)丙烯酸酯、二乙二醇單甲醚單(甲基)丙烯酸酯、二丙二醇單甲醚單(甲基)丙烯酸酯、2-乙基己基卡必醇(甲基)丙烯酸酯、(甲基)丙烯酸二環戊烯氧基乙酯、(甲基)丙烯酸二環戊烯酯、(甲基)丙烯酸三(2-羥基乙基)異氰脲酸酯、(甲基)丙烯酸苯氧基乙酯等。該等自由基聚合性單體(B)可單獨使用,亦可併用2種以上。該等之中,較佳為使用(甲基)丙烯酸甲酯、(甲基)丙烯酸二環戊烯氧基乙酯、(甲基)丙烯酸二環戊烯酯、(甲基)丙烯酸苯氧基乙酯,就進一步改善常溫乾燥性或皮膚刺激性之方面而言,尤佳為甲基丙烯酸甲酯、甲基丙烯酸二環戊烯氧基乙酯、甲基丙烯酸二環戊烯酯、甲基丙烯酸苯氧基乙酯。
關於上述自由基聚合性樹脂(A)及上述空氣乾燥性化合物(B)與上述自由基聚合性單體(C)之質量比率[(A)+(B)/(C)],就常溫乾燥性或拉伸物性等方面而言,較佳為20/80~90/10之範圍,更佳為40/60~80/20之範圍,進而較佳為50/50~70/30之範圍。
作為上述瀝青(D),可使用各種瀝青,例如可列舉:直餾瀝青、吹製瀝青、半吹製瀝青、千里達(Trinidad)瀝青、湖瀝青等。該等瀝青可單獨使用,亦可併用2種以上。
進而,作為上述瀝青(D)之含量,就賦予優異之常溫乾燥性、及防水層與瀝青鋪裝層之層間接著性之方面而言,相對於上述樹脂(A)、上述化合物(B)及上述單體(C)之合計100質量份,必需為0.01~25質量份之範圍。於上述瀝青(D)之使用量低於該範圍之情形時,無法獲得所需之層間接著性,又,於超過上述範圍之情形時,無法獲得所需之常溫乾燥性。
作為上述瀝青(D)之含量,就可進一步提高常溫乾燥性或層間接著性之方面而言,相對於上述樹脂(A)、上述化合物(B)及上述單體(C)
之合計100質量份,更佳為0.1~15質量份之範圍,更佳為0.3~10質量份之範圍,進而較佳為0.5~5質量份之範圍,尤佳為0.7~3質量份之範圍。
本發明之自由基聚合性樹脂組合物含有上述自由基聚合性樹脂(A)、上述化合物(B)、上述自由基聚合性單體(C)及上述瀝青(D),亦可視需要含有其他添加劑。
上述其他添加劑例如可使用硬化劑、硬化促進劑、抗氧化劑、防老化劑、顏料、觸變性賦予劑、溶劑、填充劑、加工處理油、塑化劑、紫外線抑制劑、補強材料、骨材、阻燃劑、穩定劑、聚合抑制劑、石油蠟等。該等之中,就可更進一步提高常溫乾燥性之方面而言,較佳為含有下述硬化劑及硬化促進劑。
作為上述硬化劑,就常溫乾燥性之方面而言,較佳為使用有機過氧化物,例如可列舉:過氧化二醯基化合物、過氧化酯化合物、氫過氧化化合物、過氧化二烷基化合物、過氧化酮化合物、過氧縮酮化合物、烷基過氧化酯化合物、過氧化碳酸酯化合物等。該等硬化劑可根據熟化條件等進行適當選擇。
作為上述硬化劑之使用量,就常溫乾燥性之方面而言,於本發明之自由基聚合性樹脂組合物中較佳為0.5~10質量%之範圍,更佳為1~5質量%之範圍。
上述硬化促進劑係具有使上述硬化劑之有機過氧化物藉由氧化還原反應而分解,從而容易產生活性自由基之作用之物質,例如可列舉:環烷酸鈷、辛酸鈷等鈷有機酸鹽,辛酸鋅、辛酸釩、環烷酸銅、環烷酸鋇等金屬皂,乙醯乙酸釩、乙醯乙酸鈷、乙醯丙酮酸鐵等金屬螯合物,苯胺、N,N-二甲基苯胺、N,N-二乙基苯胺、對甲苯胺、N,N-二甲基-對甲苯胺、N,N-二甲基-對甲苯胺之環氧乙烷加成物、N,N-雙(2-羥基乙基)對甲苯胺、4-(N,N-二甲基胺基)苯甲醛、4-[N,N-雙(2-羥
基乙基)胺基]苯甲醛、4-(N-甲基-N-羥基乙基胺基)苯甲醛、N,N-雙(2-羥基丙基)對甲苯胺、N-乙基-間甲苯胺、三乙醇胺、間甲苯胺、二伸乙基三胺、吡啶、苯基啉、哌啶、N,N-雙(羥基乙基)苯胺、二乙醇苯胺等N,N-取代苯胺、N,N-取代-對甲苯胺、4-(N,N-取代胺基)苯甲醛等胺類等。該等硬化促進劑可單獨使用,亦可併用2種以上。
作為上述硬化促進劑之使用量,就常溫乾燥性之方面而言,於本發明之自由基聚合性樹脂組合物中較佳為0.1~10質量%之範圍,更佳為0.3~5質量%之範圍。
由於本發明之自由基聚合性樹脂組合物之常溫乾燥性、及防水層與瀝青層之層間接著性優異,故而可較佳地用於自下起依序積層地板(i)、防水層(ii)、底漆層(iii)及瀝青鋪裝層(iv)而構成之地板防水結構體之底漆層(iii)。
作為上述地板(i),例如可列舉:水泥混凝土、瀝青混凝土、砂漿混凝土、樹脂混凝土、透水混凝土、ALC(Autoclaved Lightweight Concrete,熱壓養護輕質混凝土)板、PC(Polycarbonate,聚碳酸酯)板、金屬(鋼材)等。又,其形狀可為曲面、延長面、平面、傾斜面等中之任一種。亦可對上述地板(i)之表面視需要藉由公知之底漆等進行基底處理。
作為可用於上述防水層(ii)之材料,例如可使用不飽和聚酯系防水材料、環氧系防水材料、胺基甲酸酯系防水材料、聚酯系防水材料等公知之材料。
作為用於上述瀝青鋪裝層(iv)之瀝青,可使用與上述瀝青(D)相同者。
[實施例]
以下,使用實施例,對本發明更詳細地進行說明。
[合成例1]聚酯甲基丙烯酸酯(A-1)之合成
向具備溫度計、攪拌機、惰性氣體導入口、空氣導入口及回流冷卻器之四口燒瓶中添加己二酸10莫耳、二乙二醇9莫耳,並添加作為酯化觸媒之0.5質量%之氧化單丁基錫,於205℃下反應11小時。其後,冷卻至140℃,繼而投入甲基丙烯酸縮水甘油酯2莫耳,反應10小時,從而獲得數量平均分子量2,150、比重1.05之聚酯甲基丙烯酸酯(A-1)。
[合成例2]甲基丙烯酸胺基甲酸酯(A-2)之合成
向具備溫度計、攪拌機、惰性氣體導入口、空氣導入口及回流冷卻器之四口燒瓶中添加數量平均分子量1,000之聚伸丁二醇500質量份與甲苯二異氰酸酯174質量份,於氮氣氣流下、80℃下反應4小時。於異氰酸酯當量成為600即大致理論值之時刻冷卻至50℃。於空氣氣流下,加入氫醌0.07質量份,並加入甲基丙烯酸2-羥基乙酯130質量份,於90℃下反應5小時。於NCO%成為0.1質量%以下之時刻添加第三丁基兒茶酚0.07質量份,從而獲得數量平均分子量1,608之甲基丙烯酸胺基甲酸酯(A-2)。
[合成例3]空氣乾燥性化合物(B-1)之合成
向具備溫度計、攪拌機、惰性氣體導入口、空氣導入口及回流冷卻器之四口燒瓶中添加水2莫耳、二環戊二烯2莫耳,並升溫至80℃,其後滴加順丁烯二酸酐2莫耳,使其等進行反應直至酸值成為210mgKOH/g。其後,添加乙二醇1莫耳並升溫至205℃,使其等進行反應直至酸值成為20mgKOH/g,從而獲得空氣乾燥性化合物(B-1)。
[實施例1~4、比較例1~4]
[自由基聚合性樹脂組合物之製備]
以表1及2所示般將上述聚酯甲基丙烯酸酯(A-1)或甲基丙烯酸胺基甲酸酯(A-2)、上述空氣乾燥性化合物(B-1)、甲基丙烯酸甲酯及直餾瀝青進行調配,獲得自由基聚合性樹脂組合物。
[常溫乾燥性之評價方法]
常溫乾燥性係以消黏時間進行評價。具體而言,相對於實施例及比較例所獲得之自由基聚合性樹脂組合物50質量份調配8質量%辛酸鈷0.2質量份、N,N-二甲基-對甲苯胺之環氧乙烷2莫耳加成物0.15質量份、過氧化苯甲醯之漿料1質量份,利用敷料器以形成0.5mm之塗膜之方式將該調配物塗佈於25℃之玻璃板上。塗佈後,利用脫脂棉按壓塗膜表面,對直至該脫脂棉不會因黏著而殘留於塗膜表面之時間(分鐘)進行測定。再者,將未於10小時以內乾燥者設為「-」。
[層間接著性之評價方法]
相對於實施例及比較例所獲得之自由基聚合性樹脂組合物100質量份調配過氧化苯甲醯之漿料2質量份,於23℃之條件下,以2g/m塗佈於地板用防水材料(「DIOVAR VU-200」DIC股份有限公司製造)上,並使之硬化。硬化2小時後,於硬化塗膜上塗佈加熱至180℃之改質瀝青,熟化24小時,其後於23℃下根據JIS K 6854-1測定90°剝離接著強度及確認剝離狀態。
再者,將未剝離之情形評價為「A」,將自由基聚合性樹脂組合物層發生材料破損之情形評價為「B」,將確認出層間之剝離之情形評價為「C」。
得知作為本發明之自由基聚合性樹脂組合物之實施例1~4者,其常溫乾燥性、尤其是層間接著性優異。
另一方面,得知比較例1及3為不含瀝青(D)之態樣,其接著強度不足。
又,比較例2及4為瀝青(D)之含量超過本發明所規定之範圍之態樣,其常溫乾燥性明顯不良。
Claims (3)
- 一種自由基聚合性樹脂組合物,其特徵在於:其含有自由基聚合性樹脂(A)、空氣乾燥性化合物(B)、自由基聚合性單體(C)及瀝青(D),且上述瀝青(D)之含量相對於上述樹脂(A)、上述化合物(B)及上述單體(C)之合計100質量份為0.01~25質量份之範圍。
- 一種底漆,其特徵在於:其係使用如請求項1之自由基聚合性樹脂組合物而獲得。
- 一種地板防水結構體,其係自下起依序積層地板(i)、防水層(ii)、底漆層(iii)及瀝青鋪裝層(iv)而構成者,其特徵在於:上述底漆層(iii)係使用如請求項2之底漆而獲得。
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