JP6740101B2 - 難燃性組成物及びそれを含む難燃性基材並びに難燃性基材の製造方法 - Google Patents
難燃性組成物及びそれを含む難燃性基材並びに難燃性基材の製造方法 Download PDFInfo
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Description
本発明の難燃性組成物は、ホウ酸、ホウ砂及び次の化学式(1)で表されるビニルホスホン酸ジアルキルポリマーを含有するもの(以下、「本発明組成物」という)である。
本発明の難燃性基材は、本発明組成物と基材とを含むもの(以下、「本発明難燃性基材」という)である。
下記参考例1および参考例2において得られたポリマーの重量平均分子量(Mw)及び分子量分布(Mw/Mn)は、ゲルパーミエイションクロマトグラフィ(GPC)により測定し、標準ポリエチレンオキサイド試料を用いた換算値から算出した。
GPC測定装置:SHIMADZU社製LC−Solution
カラム:Shodex SB−805HQ、Shodex SB−804HQ
プレカラム:Shodex SB−G
カラム温度:40℃
移動相:0.2M NaCl水溶液
流量:0.5mL/min
検出器:RI検出器
(参考例1)ビニルホスホン酸ジメチルポリマー:
10L反応装置を窒素置換し、ヘキサンを2479g投入した。撹拌しながら、反応溶液を70℃まで昇温後、ビニルホスホン酸ジメチルモノマーを2760g(丸善石油化学社製)、重合開始剤(V−601(和光純薬工業社製))を280g投入した。その後、8hr反応することで、ビニルホスホン酸ジメチルポリマーを合成した。反応溶液を室温まで冷却後、イオン交換水を2760g投入した。十分撹拌した後、ビニルホスホン酸ジメチルポリマー水溶液を抜出し、濃縮することで、50wt%のポリマー水溶液を得た。
得られたポリマーの分子量は、GPCによる分析結果から、重量平均分子量Mw5600、分子量分布Mw/Mn2.71となった。
(参考例2)ビニルホスホン酸ポリマー:
10L反応装置を窒素置換し、イオン交換水を3162g、ビニルホスホン酸モノマーを5080g投入した。撹拌しながら、反応溶液を80℃まで昇温後、イオン交換水を1743g、重合開始剤(V−50(和光純薬工業社製))を383g投入した。その後、7hr反応することで、ビニルホスホン酸ポリマーを合成した。合成したポリマー水溶液の濃度は、50wt%であった。
得られたポリマーの分子量は、GPCによる分析結果から、重量平均分子量Mw9100、分子量分布Mw/Mn1.95となった。
(実施例1)
1500mLのビーカーにイオン交換水を413g投入し、ホウ酸を240g、ホウ砂を299g、50wt%濃度の参考例1で合成したビニルホスホン酸ジメチルポリマー水溶液を300g(ビニルホスホン酸ジメチルポリマーとして150g)投入し、60℃で、混合溶液を十分に撹拌した。その後、濁りのない清澄な溶液を得た。
1500mLのビーカーにイオン交換水を602g投入し、ホウ酸を240g、ホウ砂を299g添加し、60℃に昇温し、混合溶液を十分に撹拌した。その後、濁りのない清澄な溶液を得た。
1000mLのビーカーにイオン交換水を602g投入し、ホウ酸を120g、ホウ砂を150g添加し、60℃に昇温し、混合溶液を十分に撹拌した。その後、濁りのない清澄な溶液を得た。
1500mLのビーカーにイオン交換水を506g投入し、ホウ酸を201g、ホウ砂を250g、50wt%濃度の参考例2で合成したビニルホスホン酸ポリマー水溶液を507g(ビニルホスホン酸ポリマーとして253.5g)添加し、90℃に昇温し、混合溶液を十分に撹拌した。その後、濁りのない清澄な溶液を得た。
実施例1の難燃性組成物及び比較例1〜3の比較組成物に、40mm×40mm×40mmに裁断した杉材(絶乾比重0.26〜0.31)をそれぞれ投入し、オートクレーブにより、1MPa、60℃以上、24時間、加圧加熱処理を行った。その後、115℃で40時間以上乾燥処理を行った。上記組成物の含浸前の杉材の重量と、含浸乾燥後の杉材の重量から、含浸率を求めた。また、得られた杉材について、以下の燃焼試験および白華試験を行った。これら結果を組成とともに表1に示す。
上記、難燃性組成物の含浸乾燥処理を施した杉材を750℃に保持したマッフル炉で20分間加熱し、その際の重量減少率から難燃性を評価した。
ここで、建築基準法に基づく不燃認定を受けるためには、不燃試験および燃焼試験のいずれかに合格する必要がある。不燃試験は、直径40mm、高さ55mmの円柱状の木材片を750℃のマッフル炉の中に20分間保持して、重量減少率を調べるもので、重量減少率が30%以下となることが合格の必要条件となる。また、燃焼試験は、コーンカロリーメータで火災初期に相当する熱を試料に与えたときの20分間における総発熱量が8MJ/m2以下であることが合格の必要条件となる。一般に、前者の条件は後者の条件よりも厳しく、後者の条件を満たす総発熱量8MJ/m2の試料は前者の試験において、重量減少率が約44%を示す。すなわち、750℃で20分間加熱したときの重量減少率が44%以下であれば、不燃の条件を満たす可能性が高い。
白華現象の評価は、目視により基材の表面に現れた白華の有無を確認して行った。
Claims (7)
- ビニルホスホン酸ジアルキルポリマーが、ビニルホスホン酸ジメチルポリマーである請求項1に記載の難燃性組成物。
- 基材が木材、紙、織物、不織布および樹脂から選択される何れかである請求項4記載の難燃性基材の製造方法。
- 基材が木材である請求項4記載の難燃性基材の製造方法。
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