JP2020509145A - ポリウレタンフォームおよびその製造方法 - Google Patents
ポリウレタンフォームおよびその製造方法 Download PDFInfo
- Publication number
- JP2020509145A JP2020509145A JP2019548735A JP2019548735A JP2020509145A JP 2020509145 A JP2020509145 A JP 2020509145A JP 2019548735 A JP2019548735 A JP 2019548735A JP 2019548735 A JP2019548735 A JP 2019548735A JP 2020509145 A JP2020509145 A JP 2020509145A
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- Prior art keywords
- component
- isocyanate
- weight
- polyol
- reaction mixture
- Prior art date
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- C08G18/48—Polyethers
- C08G18/4825—Polyethers containing two hydroxy groups
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- C08G18/1841—Catalysts containing secondary or tertiary amines or salts thereof having carbonyl groups which may be linked to one or more nitrogen or oxygen atoms
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- B29C41/00—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor
- B29C41/003—Shaping by coating a mould, core or other substrate, i.e. by depositing material and stripping-off the shaped article; Apparatus therefor characterised by the choice of material
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- B29C44/10—Applying counter-pressure during expanding
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
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- C—CHEMISTRY; METALLURGY
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- C08G18/667—Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
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Abstract
Description
i)ポリオール配合物P)を含む発泡性反応混合物R)を製造する工程であって、
−イソシアネート反応性成分A)であって、前記イソシアネート反応性成分A)は、ポリエーテルポリオール、ポリエステルポリオール、ポリカーボネートポリオール、ポリエーテルポリカーボネートポリオールおよびポリエーテルエステルポリオールからなる群から選択される>2.5の官能基数fを有する少なくとも1種のポリオール成分A1)を含んでなる、イソシアネート反応性成分A)と
−ツェレウィチノフ活性水素を有する触媒活性成分D1)を少なくとも含有する触媒成分D)と、
−気泡連通化化合物を少なくとも含んでなる助剤および添加剤物質E)と、を含み、
成分A)における末端OH官能基の総数に対してイソシアネート反応性成分A)中に存在する全第一級OH官能基の比率は、少なくとも30%である、前記ポリオール配合物P)と、
ポリイソシアネート成分B)と、
発泡剤成分C)として超臨界状態のCO2と、
を含む、前記発泡性反応混合物R)を製造する工程と、
ii)型に発泡性反応混合物R)を導入する工程と、
iii)反応混合物R)を発泡させる工程と、
iv)硬質PUR/PIRフォームを脱型する工程と、
を含んでなる方法を提供する。
イソシアネート指数(指数としても知られる)は、イソシアネート基の実際に使用された物質量[モル]およびイソシアネート反応性基の実際に使用された物質量[モル]の商を100で乗じたものを意味すると理解されるものとする:
指数=(イソシアネート基のモル数/イソシアネート反応性基のモル数)*100。
工程ii)の終了後、1〜40秒、特に好ましくは5〜20秒、非常に特に好ましくは8〜17秒である期間1の間、型内の圧を一定に保持し、最初、発泡しないで、反応混合物の粘度は増大する。好ましい期間の間、圧を保持することは、この反応区間に対して混合物の特に有利な粘度範囲をもたらすと分かった。期間1が経過した時点で、型を減圧する。1〜90バール/秒、好ましくは1〜80バール/秒、特に好ましくは2〜70バール/秒の圧力開放速度で、型の圧力開放を期間2にわたって行う。 特に比例弁により開放を行うことができる。反応混合物を期間2にわたって発泡する。過剰に迅速な開放は、気泡安定性に悪影響を及ぼし、過剰に遅い開放は発泡反応に悪影響を及ぼす。
i)発泡性反応混合物R)を製造する工程であって、
− >2.5のOH官能基数を有する、ポリエーテルポリオール、ポリエステルポリオール、ポリカーボネートポリオールおよびポリエーテルポリカーボネートポリオールおよびポリエーテルエステルポリオールからなる群から選択される少なくとも1種のポリオール成分A1)を含有するイソシアネート反応性成分A)と、
− 少なくとも1種のポリイソシアネート成分B)と、
− 少なくとも1種の発泡剤C)と、
− ツェレウィチノフ活性水素を有する触媒活性成分D1)を少なくとも含有する触媒成分D)と、
− 気泡連通化化合物を少なくとも含んでなる助剤および添加剤物質E)と、
成分A)における末端OH官能基の総数に対してイソシアネート反応性成分A)中に存在する全第一級OH官能基の比率は、少なくとも30%である、
から発泡性反応混合物R)を製造する工程と、
ii)成分A)、発泡剤およびポリイソシアネート成分B)からなる発泡性反応混合物を、封止型に導入する工程であって、注入中の型における反対圧力は2〜90バールである工程と、
iii)工程ii)の終了後、型内の圧を、1〜40秒の期間1の間、保持し、その後、1〜90バール/秒の圧力開放速度で、期間2にわたって型から圧を開放する工程と、
iv)硬質PUR/PIRフォームを脱型する工程と、
を含む。
かさ密度の決定:ゴムおよびプラスチックからなる発泡体 − かさ密度の決定(ISO845:2006);独国版EN ISO845:2009。
連続気泡率の決定:連続および独立気泡の容積分率の決定(ISO4590:2002);独国版EN ISO4590:2003。
圧縮強さの決定:硬質発泡体 − 圧特性の決定(ISO844:2014);独国版EN ISO844:2014。
OH価の決定:水酸基価の決定 − パート2:2007年11月版のDIN53240−2に従った触媒を用いた方法。
気泡サイズの決定:VHX5000光学顕微鏡による光学顕微鏡評価;測定しようとする検体をいずれの場合にも5mmの径を有する円領域にわたって3つの異なる点において分析する。選択された領域が約100個の気泡を得るように解像度を選択する。それから、100個の気泡を測定し、最小および最大の気泡直径ならびに平均気泡直径を算出する。
表1中の第一級OH官能基の詳細な比率[%]は、配合物中に存在するポリオールの混合物のOH官能基の総数に対する第一級OH官能基の比率に関する。
CO2およびn−ペンタンで発泡したポリウレタンフォームを、次の表1に記載された配合物により製造した。報告された数は、特に指定されない限り、重量部を意味すると理解されるものとする。次の物質を使用した:
実験室でフリーライズポリウレタンフォームを製造するため、下表1に挙げられたポリオール、安定剤および触媒からなるそれぞれのポリオール配合物さらに発泡剤の組成物200gを製造した。反応混合物を製造するため、ポリオール配合物および発泡剤からなるこの組成物を、Pendraulik撹拌機を用いて対応する量のイソシアネートと23℃において10秒間混合し、開口型(20cm×20cm×18cm)に注いだ。正確な配合を表1に纏めており、反応混合物特性および発泡体の物理的試験の結果を表2に纏めている。
実験室で成形ポリウレタンフォームを製造するため、下表1に挙げられたポリオール、安定剤および触媒からなるそれぞれのポリオール配合物さらに発泡剤の組成物100gを製造した。反応混合物を製造するため、ポリオール配合物および発泡剤からなるこの組成物を、Pendraulik撹拌機を用いて対応する量のイソシアネートと23℃において10秒間混合し、型(20cm×20cm×6cm)に注いだ。注ぎ入れた直後に型を密閉した。したがって、このように製造された成形物品を5分後に脱型した。正確な配合を表1に纏めており、発泡体の物理的試験の結果を表2に纏めている。
高圧プラントにおいてフリーライズポリウレタンフォームを製造するため、下表1に挙げられたポリオール、安定剤および触媒からなるポリオール配合物を製造した。標準的高圧混合プラントにおいてポリオール成分としてこれを使用し、150バールの圧および50℃の温度において発泡剤CO2と混合した。したがって、ここで、発泡剤は超臨界条件下であった。高圧ミキシングヘッドでは、この混合物を、150バールの圧および35℃の温度において運搬されたイソシアネートと混合した。ショット量は、48ml/秒の体積流量に対応する40g/秒であった(混合物密度1.2g/ml)。このように得られた反応混合物を、50℃の型温度において10バールの反対圧力で圧縮応力を与えられた封止型(1lの体積を有する)に注入した。注入終了後、10バールの圧縮応力を与えられた反対圧力をさらに12秒間維持し、それから<2秒を通して周囲圧力まで減圧した。このように製造された成形物品を、5分後に脱型した。正確な配合を表1に纏めており、発泡体の物理的試験の結果を表2に纏めている。
Claims (13)
- 硬質PUR/PIRフォームを製造する方法であって、前記硬質PUR/PIRフォームが、ISO845:2006に従って30〜90kg/m3、好ましくは30〜70kg/m3のかさ密度を有し、ISO4590:2002に従って>90%、好ましくは≧94%の連続気泡率を有し、光学顕微鏡評価により<50μmの平均気泡直径を有するものであり、該方法が:
i)本発明の反応混合物R)を製造する工程であって、該反応混合物R)が:
ポリオール配合物P)であって、該ポリオール配合物P)が:
−イソシアネート反応性成分A)であって、該イソシアネート反応性成分A)が、ポリエーテルポリオール、ポリエステルポリオール、ポリカーボネートポリオール、ポリエーテルポリカーボネートポリオールおよびポリエーテルエステルポリオールからなる群から選択される、>2.5の官能基数fを有する少なくとも1種のポリオール成分A1)を含んでなる、イソシアネート反応性成分A)と、
−ツェレウィチノフ活性水素を有する触媒活性成分D1)を少なくとも含有する触媒成分D)と、
−気泡連通化化合物を少なくとも含んでなる助剤および添加剤物質E)と、を含み、
イソシアネート反応性成分A)における末端OH官能基の総数に対して、成分A)中に存在する全第一級OH官能基の比率が少なくとも30%である、ポリオール配合物P)と、
ポリイソシアネート成分B)と、
発泡剤成分C)として超臨界状態のCO2と、
を含む、本発明の反応混合物R)を製造する工程、
ii)型に前記発泡性反応混合物R)を導入する工程、
iii)前記反応混合物R)を発泡させる工程、ならびに
iv)硬質PUR/PIRフォームを脱型する工程、
を含んでなる、方法。 - 工程i)および必要に応じて工程ii)を、超臨界条件下で行う、請求項1に記載の方法。
- 工程i)を、ミキシングヘッドまたは高圧ミキシングヘッドにおいて行う、請求項1または2に記載の方法。
- 工程ii)において、成分A)、発泡剤C)およびポリイソシアネート成分B)からなる発泡性反応混合物R)が封止型に導入され、注入中の前記型における反対圧力が2〜90バールであることを特徴とする、請求項1〜3のいずれか一項に記載の方法。
- 工程ii)において、成分A)、発泡剤T)およびポリイソシアネート成分B)からなる発泡性反応混合物R)が封止型に導入され、注入中の前記型における反対圧力が2〜90バールであり、かつ
工程iii)において、工程ii)の終了後、前記型内の前記圧が、1〜40秒の期間1の間維持され、その後、1〜90バール/秒の圧力開放速度で、期間2にわたって前記型から前記圧が開放される
ことを特徴とする、請求項1に記載の方法。 - 前記ポリオール成分A1)が280〜600mg KOH/gの水酸基価(DIN53240−2(2007))を有することを特徴とする、請求項1に記載の方法。
- 前記イソシアネート反応性成分A)が、少なくとも65重量%の程度の、280〜600mg KOH/gの水酸基価および≧2.8〜≦6.0の官能基数を有する前記ポリオール成分A1)からなり、前記成分A)における第一級OH官能基の比率が少なくとも35%(前記成分Aにおける全末端OH官能基に対して)であることを特徴とする、請求項1に記載の方法。
- イソシアネート反応性成分A)が、少なくとも60重量%の程度のポリエーテルポリオールからなることを特徴とする、請求項1に記載の方法。
- 気泡連通化化合物E)の含有率が、0.1〜1.0重量%であることを特徴とする、請求項1に記載の方法。
- それが、前記成分A)の総重量に対して≧0.01重量%〜<2重量%の量で触媒活性化合物D1)を含有することを特徴とする、請求項1に記載の方法。
- 発泡剤成分C)の含有率が、R)の総重量に対して0.5重量%〜15重量%である、請求項1に記載の方法。
- 請求項1〜11のいずれか一項に記載の方法によって得られる、連続気泡硬質PUR/PIRフォーム。
- 請求項12に記載の硬質PUR/PIRフォームを含む、冷蔵庫、冷凍庫または冷凍冷蔵庫。
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- 2018-03-05 CN CN201880016564.0A patent/CN110382581A/zh active Pending
- 2018-03-05 CN CN201880016566.XA patent/CN110382582A/zh active Pending
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WO2018162387A1 (de) | 2018-09-13 |
EP3592791A1 (de) | 2020-01-15 |
EP3372625A1 (de) | 2018-09-12 |
HUE060122T2 (hu) | 2023-01-28 |
US11168172B2 (en) | 2021-11-09 |
PL3592791T3 (pl) | 2022-12-19 |
CN110382582A (zh) | 2019-10-25 |
US20200080767A1 (en) | 2020-03-12 |
CN110382581A (zh) | 2019-10-25 |
EP3592791B1 (de) | 2022-08-17 |
WO2018162372A1 (de) | 2018-09-13 |
EP3592790A1 (de) | 2020-01-15 |
US20200017624A1 (en) | 2020-01-16 |
JP7110221B2 (ja) | 2022-08-01 |
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