JP2019529622A - 採鉱における空洞を充填するための火炎伝播しないポリアミドフォーム - Google Patents
採鉱における空洞を充填するための火炎伝播しないポリアミドフォーム Download PDFInfo
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- JP2019529622A JP2019529622A JP2019512818A JP2019512818A JP2019529622A JP 2019529622 A JP2019529622 A JP 2019529622A JP 2019512818 A JP2019512818 A JP 2019512818A JP 2019512818 A JP2019512818 A JP 2019512818A JP 2019529622 A JP2019529622 A JP 2019529622A
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- JP
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- Prior art keywords
- isocyanate
- acid
- reactive
- component
- foam
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
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Abstract
Description
本発明は、火炎伝播しないポリアミドフォームの製造方法、ならびに採鉱、トンネル工事、土木工事におけるまたは石油採取およびガス採取における空洞の充填方法に関する。
(i)少なくとも1つのポリイソシアナートを含み、かつ芳香族イソシアナート基の、芳香族イソシアナート基および脂肪族イソシアナート基の合計に対するモル比が、少なくとも60モル%である、液体のイソシアナート成分を、
(ii)反応性希釈剤を含み、かつこの反応性希釈剤は、
(a)分枝した脂肪族C24〜C66−ポリカルボン酸、脂環式C24〜C66−ポリカルボン酸、および少なくとも2つのエステル化されていないカルボキシル基を有するポリカルボン酸の部分エステルの中から選択される連鎖延長する反応性希釈剤および/または架橋する反応性希釈剤、および/または
(b)分枝した脂肪族C24〜C66−モノカルボン酸、脂環式C24〜C66−モノカルボン酸、および1つのエステル化されていないカルボキシル基を有するポリカルボン酸の部分エステルの中から選択される連鎖停止する反応性希釈剤、
を含む少なくとも1つの液体のイソシアナート反応性成分、および
(iii)場合により固体のイソシアナート反応性成分とを
混合することによる火炎伝播しないポリアミドフォームの製造方法において、液体のイソシアナート反応性成分および/または固体のイソシアナート反応性成分は、芳香族C8〜C18−ポリカルボン酸および/またはその無水物を含む、火炎伝播しないポリアミドフォームの製造方法により解決される。
1.芳香族、脂肪族および/または脂環式ジイソシアナートの、イソシアヌラート基を有するポリイソシアナート。この場合に存在するイソシアヌラートは、ことにジイソシアナートの環状三量体、またはその高級の、1つより多いイソシアヌラート環を有する同族体との混合物である。
2.芳香族、脂肪族および/または脂環式に結合したイソシアナート基を有するウレトジオンジイソシアナート。ウレトジオンジイソシアナートは、ジイソシアナートの環式二量体生成物である。
3.芳香族、脂肪族または脂環式に結合したイソシアナート基を有する、ビウレット基を有するポリイソシアナート。
4.芳香族、脂肪族または脂環式に結合したイソシアナート基を有する、ウレタン基および/またはアロファナート基を有するポリイソシアナート、例えばこれは、過剰量のジイソシアナートと、多価アルコール、例えばトリメチロールプロパン、ネオペンチルグリコール、ペンタエリトリット、1,4−ブタンジオール、1,6−ヘキサンジオール、1,3−プロパンジオール、エチレングリコール、ジエチレングリコール、グリセリン、1,2−ジヒドロキシプロパンまたはこれらの混合物との反応により得ることができる。
5.オキサジアジントリオン基含有ポリイソシアナート。
6.ウレトンイミン変性されたポリイソシアナート。
(a)アミノ基含有オリゴマーまたはポリマーのリン酸エステル塩、例えば場合により脂肪酸変性されたまたはアルコキシル化された(ことにエトキシル化された)ポリアミンのリン酸エステル塩、エポキシド−ポリアミン付加物のリン酸エステル塩、アミノ基含有アクリラートコポリマーまたはメタクリラートコポリマーのリン酸エステル塩、およびアクリラート−ポリアミン付加物のリン酸エステル塩、
(b)リン酸のモノエステルまたはジエステル、例えばリン酸のアルキル−、アリール−、アラルキル−またはアルキルアリール−アルコキシラートとのモノエステルまたはジエステル(例えばノニルフェノールエトキシラート、イソトリデシルアルコールエトキシラート、ブタノールにより開始されたアルキレンオキシドポリエーテルのリン酸モノエステルまたはリン酸ジエステル)、リン酸とポリエステルとのモノエステルまたはジエステル(例えばラクトンポリエステル、例えばカプロラクトンポリエステルまたは混合型のカプロラクトン/バレロラクトン−ポリエステル)、
(c)酸性のジカルボン酸半エステル、例えばアルキル−、アリール−、アラルキル−またはアルキルアリール−アルコキシラート(例えばノニルフェノールエトキシラート、イソトリデシルアルコールエトキシラートまたはブタノールにより開始されたアルキレンオキシドポリエーテル)との酸性のジカルボン酸半エステル(ことにコハク酸、マレイン酸またはフタル酸)、
(d)ポリウレタン−ポリアミン付加物、
(e)ポリアルコキシル化されたモノアミンまたはジアミン(例えばエトキシル化されたオレイルアミンまたはアルコキシル化されたエチレンジアミン)、
(f)不飽和脂肪酸の、モノアミン、ジアミンおよびポリアミンとの反応生成物、アミノアルコール、および不飽和1,2−ジカルボン酸およびその無水物、およびその塩、およびアルコールおよび/またはアミンとの反応生成物。
Lupranat M10R(BASF)ポリマーのメチレンジフェニルイソシアナート(NCO含有率31.7%、公称NCO官能価2.2)
Lupranat M20R(BASF)ポリマーのメチレンジフェニルイソシアナート(NCO含有率31.4%、公称NCO官能価2.7)
Lupranat M200R(BASF)ポリマーのメチレンジフェニルイソシアナート(NCO含有率31%、公称NCO官能価3)
Jeffcat ZR 50(Huntsman)N,N−ビス(3−ジメチルアミノプロピル)−N−イソプロパノールアミン
Jeffcat ZR 70(Huntsman)2−(2−ジメチルアミノエトキシ)エタノール
Lupragen N106(BASF)4,4−(オキシジ−2,1−エタンジイル)ビスモルホリン
Lupragen N201(BASF)ジアザビシクロオクタン
Lupragen N600(BASF)1,3,5−トリス(ジメチルアミノプロピル)−sym−ヘキサヒドロトリアジン
Lupragen TCPP(BASF)トリクロロプロピルホスファート
Empol 1062(BASF)トール油を基礎とする脂肪酸二量体(蒸留、部分的に水素化)
Empol 1043(BASF)トール油を基礎とする脂肪酸三量体
Pripol 1017(Croda)脂肪酸二量体(酸価190〜197mgKOH/g)
Pripol 1040(Croda)脂肪酸三量体(酸価184〜194mgKOH/g)
Tegostab B 8407(Evonik)ポリオキシアルキレンポリシロキサン
成分1:Lupranat M20R 6g
成分2:Empol 1062 5gおよびJeffcat ZR 70 0.5g
成分2.1:イソフタル酸1.2g
成分1:Lupranat M20R 6g
成分2:Empol 1062 5gおよびJeffcat ZR 70 0.5gおよびイソフタル酸(トリエチルホスファート4g中に予め溶解)1.2g
成分1:Lupranat M20R 6g
成分2:Empol 1062 5gおよびJeffcat ZR 70 0.5gおよびTegostab B 8407 0.2gおよびイソフタル酸(この中に分散)1.2g
成分1:Lupranat M20R 6g
成分2:Empol 1043 4.5gおよびJeffcat ZR 70 0.5g
成分2.1:テレフタル酸1.2g
成分1:Lupranat M10R 6g
成分2:Empol 1043 4.5gおよびJeffcat ZR 70 0.5gおよびTegostab B 8407 0.2g
成分2.1:イソフタル酸1.2g
実施例5に従って、70kg/m3の密度を有するフォーム片を製造した。このフォーム片から得られた角柱を、機械的圧縮試験にかけた。10%の圧縮率で0.2N/mm2の平均圧縮強さが得られた。
実施例5に従って、75kg/m3の密度を有するフォーム片を製造した。このフォーム片から得られた20×20×4cmの寸法を有するプレートを、その熱伝導率に関して調査した。これは、51mW/(m・K)の熱伝導率を有する。
実施例5により製造されたフォーム片を、熱重量分析により調査した。フォームの分解は420℃の温度で始まった。
実施例5に従って、4倍量の触媒(残りの成分の全体量に対して)および硬化可能な混合物200gの製造のための高めたバッチサイズを有するバッチを、反応熱の調査のために実施した。30℃の予熱したこれらの成分を混合し、発泡過程の間の反応温度を測定した。最大反応温度は50℃であった。
成分1:Lupranat M10R 6g
成分2:Pripol 1017 4g、Pripol 1040 2gおよび水0.6gおよび4,4−(オキシジ−2,1−エタンジイル)ビスモルホリン(Lupragen N106)1gおよびTegostab B 8407 0.5g
第一の成分を第二の成分と14秒間混合した後、混合物は発泡し始める。発泡過程は、14倍の体積増加で2分後に完了する。実施例1〜5のフォームとは反対に、極めて微細なフォーム構造を有する不粘着性の固体のフォームが生じる。
成分1:Lupranat M10R 6g
成分2:Pripol 1017 4g、Pripol 1040 2gおよび水0.6gおよび4,4−(オキシジ−2,1−エタンジイル)ビスモルホリン(Lupragen N106)1gおよびTegostab B 8407 0.5g
成分2.1:イソフタル酸1.2g
実施例1〜5のフォームとは反対に、このフォームは、極めて微細なフォーム構造を有する。
成分1:Lupranat M20R 6g
成分2:Pripol 1017 2g、Pripol 1040 4g、水0.6g、4,4−(オキシジ−2,1−エタンジイル)ビスモルホリン(Lupragen N106)0.15g、Jeffcat ZR50 1.0g、Tegostab B 8407 0.5gおよびイソフタル酸(この中に均一に分散)3g
得られたフォームは、実施例1〜5よりも微細なフォーム構造を有する。この配合により製造されたフォーム片は、実施例9と同様に、BS5946:1980によるパンキング試験にかけた。この発泡体は試験に合格した。実施例10および11のフォームと比較して、このフォームはより良好な火炎挙動を示し、つまりこのフォームは、困難に引火可能で、自己消火性で、炭化および溶融しがたい。
成分1:Lupranat M20R 6g
成分2:Pripol 1017 2g、Pripol 1040 4g、水0.6g、4,4−(オキシジ−2,1−エタンジイル)ビスモルホリン(Lupragen N106)0.15g、Jeffcat ZR50 1.0g、Tegostab B 8407 0.5g、イソフタル酸2gおよびトリメリト酸1g(この中に均一に分散)
得られたフォームは、実施例1〜5よりも微細なフォーム構造を有するが、実施例10および11よりも良好な火炎挙動(困難に引火可能、自己消火性、炭化および溶融しがたい)を示す。
ポリアミドフォームは、次の表にまとめられた成分および使用量(gで表される)から、次のように製造した:Lupranat N200Rを除く全ての成分を混合し、次いでLupranat N200Rを混ぜ合わせた。この混合物は発泡し、硬化後に固体のポリアミドフォームを形成する。フォーム片から、24時間後に、12×12×12cm3のサイズの立方体を切り出した。立方体の火炎挙動を、実施例9に記載されたパンキング試験で調査した。10分後または20分後に達成された温度T1(底部)およびT2(中央部)も、同様に表中に示されている。
Claims (14)
- (i) 少なくとも1つのポリイソシアナートを含み、かつ芳香族イソシアナート基の、芳香族イソシアナート基および脂肪族イソシアナート基の合計に対するモル比が、少なくとも60モル%である、液体のイソシアナート成分を、
(ii)反応性希釈剤を含み、かつ前記反応性希釈剤は、
(a)分枝した脂肪族C24〜C66−ポリカルボン酸、脂環式C24〜C66−ポリカルボン酸、および少なくとも2つのエステル化されていないカルボキシル基を有するポリカルボン酸の部分エステルの中から選択される連鎖延長する反応性希釈剤および/または架橋する反応性希釈剤、および/または
(b)分枝した脂肪族C24〜C66−モノカルボン酸、脂環式C24〜C66−モノカルボン酸、および1つのエステル化されていないカルボキシル基を有するポリカルボン酸の部分エステルの中から選択される連鎖停止する反応性希釈剤
を含む少なくとも1つの液体のイソシアナート反応性成分、および
(iii)場合により固体のイソシアナート反応性成分とを混合することによる火炎伝播しないポリアミドフォームの製造方法において、
前記液体のイソシアナート反応性成分および/または前記固体のイソシアナート反応性成分は、芳香族C8〜C18−ポリカルボン酸および/またはその無水物を含む、火炎伝播しないポリアミドフォームの製造方法。 - 前記液体のイソシアナート成分は、ジフェニルメタンジイソシアナート、モノマーのジフェニルメタンジイソシアナートとジフェニルメタンジイソシアナートの多環式同族体との混合物またはジフェニルメタンジイソシアナートのプレポリマー、またはこれらの混合物を含むことを特徴とする、請求項1記載の方法。
- 前記分枝した脂肪族C24〜C66−ポリカルボン酸および/または脂環式C24〜C66−ポリカルボン酸は、場合により水素化されている二量体脂肪酸、三量体脂肪酸およびこれらの混合物の中から選択されることを特徴とする、請求項1または2記載の方法。
- (ii)および(iii)中の芳香族カルボキシル基の、芳香族カルボキシル基と脂肪族カルボキシル基との合計に対するモル比は、少なくとも10モル%であることを特徴とする、請求項1から3までのいずれか1項記載の方法。
- 前記液体のイソシアナート成分、前記液体のイソシアナート反応性成分および/または前記固体のイソシアナート反応性成分は、重付加触媒を含むことを特徴とする、請求項1から4までのいずれか1項記載の方法。
- 前記重付加触媒は、有機スズ化合物、第三級アミンおよびアルカリ土類金属塩の中から選択されることを特徴とする、請求項5記載の方法。
- 前記液体のイソシアナート成分および/または前記液体のイソシアナート反応性成分は、起泡安定剤を含むことを特徴とする、請求項1から6までのいずれか1項記載の方法。
- 前記液体のイソシアナート成分、前記液体のイソシアナート反応性成分および/または前記固体のイソシアナート反応性成分は、難燃剤を含むことを特徴とする、請求項1から7までのいずれか1項記載の方法。
- 火炎伝播しないポリアミドフォームによる、採鉱、トンネル工事、土木工事におけるまたは石油採取およびガス採取における空洞の充填方法において、請求項1に定義された前記液体のイソシアナート成分、前記液体のイソシアナート反応性成分および場合により前記固体のイソシアナート反応性成分を混合し、混合物を前記空洞内に導入する、空洞の充填方法。
- 前記空洞は型枠で限定されていて、かつ前記混合物を限定された空洞内へ導入することを特徴とする、請求項9記載の方法。
- 請求項1から8までのいずれか1項記載の方法により得られるポリアミドフォーム。
- 請求項11記載のポリアミドフォームの防火フォームとしての使用。
- 請求項11記載のポリアミドフォームの断熱材としての使用。
- 請求項11記載のポリアミドフォームの遮音材としての使用。
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TW201634514A (zh) | 2015-02-05 | 2016-10-01 | 羅傑斯公司 | 發泡體產物及其製備方法 |
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- 2017-09-04 WO PCT/EP2017/072096 patent/WO2018046437A1/de unknown
- 2017-09-04 US US16/326,869 patent/US11130834B2/en active Active
- 2017-09-04 ES ES17758893T patent/ES2821921T3/es active Active
- 2017-09-04 CA CA3035447A patent/CA3035447A1/en active Pending
- 2017-09-04 AU AU2017323407A patent/AU2017323407B2/en active Active
- 2017-09-04 JP JP2019512818A patent/JP7003115B2/ja active Active
- 2017-09-04 CN CN201780051785.7A patent/CN109642014B/zh active Active
- 2017-09-04 EP EP17758893.6A patent/EP3510072B1/de active Active
- 2017-09-04 RS RS20201130A patent/RS60876B1/sr unknown
- 2017-09-04 PL PL17758893T patent/PL3510072T3/pl unknown
- 2017-09-04 PT PT177588936T patent/PT3510072T/pt unknown
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Publication number | Publication date |
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EP3510072A1 (de) | 2019-07-17 |
CN109642014B (zh) | 2021-11-05 |
JP7003115B2 (ja) | 2022-02-04 |
ES2821921T3 (es) | 2021-04-28 |
PT3510072T (pt) | 2020-09-25 |
AU2017323407B2 (en) | 2021-10-07 |
RS60876B1 (sr) | 2020-11-30 |
CA3035447A1 (en) | 2018-03-15 |
EP3510072B1 (de) | 2020-06-24 |
WO2018046437A1 (de) | 2018-03-15 |
US20190211137A1 (en) | 2019-07-11 |
PL3510072T3 (pl) | 2020-11-30 |
AU2017323407A1 (en) | 2019-04-04 |
US11130834B2 (en) | 2021-09-28 |
CN109642014A (zh) | 2019-04-16 |
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