JP4952982B2 - 湿気硬化性ポリウレタンホットメルト樹脂及び粒子状物質の混合方法 - Google Patents
湿気硬化性ポリウレタンホットメルト樹脂及び粒子状物質の混合方法 Download PDFInfo
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- JP4952982B2 JP4952982B2 JP2006170002A JP2006170002A JP4952982B2 JP 4952982 B2 JP4952982 B2 JP 4952982B2 JP 2006170002 A JP2006170002 A JP 2006170002A JP 2006170002 A JP2006170002 A JP 2006170002A JP 4952982 B2 JP4952982 B2 JP 4952982B2
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- polyurethane hot
- hot melt
- melt resin
- moisture
- curable polyurethane
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- 229910052613 tourmaline Inorganic materials 0.000 description 1
- 239000011032 tourmaline Substances 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- HQUQLFOMPYWACS-UHFFFAOYSA-N tris(2-chloroethyl) phosphate Chemical compound ClCCOP(=O)(OCCCl)OCCCl HQUQLFOMPYWACS-UHFFFAOYSA-N 0.000 description 1
- NWIKMSABBNGQRG-UHFFFAOYSA-N tris(3,3-dibromopropyl) phosphate Chemical compound BrC(Br)CCOP(=O)(OCCC(Br)Br)OCCC(Br)Br NWIKMSABBNGQRG-UHFFFAOYSA-N 0.000 description 1
- XHTMGDWCCPGGET-UHFFFAOYSA-N tris(3,3-dichloropropyl) phosphate Chemical compound ClC(Cl)CCOP(=O)(OCCC(Cl)Cl)OCCC(Cl)Cl XHTMGDWCCPGGET-UHFFFAOYSA-N 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
- BIKXLKXABVUSMH-UHFFFAOYSA-N trizinc;diborate Chemical compound [Zn+2].[Zn+2].[Zn+2].[O-]B([O-])[O-].[O-]B([O-])[O-] BIKXLKXABVUSMH-UHFFFAOYSA-N 0.000 description 1
- 238000011077 uniformity evaluation Methods 0.000 description 1
- 239000001993 wax Substances 0.000 description 1
- 239000012463 white pigment Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 239000002759 woven fabric Substances 0.000 description 1
Landscapes
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Description
より具体的には、粒子状物質が均一分散していない組成物を、例えば前記合成皮革等の表皮層の形成に使用した場合には、表皮層の色むらや色分かれ、隠蔽性の低下等を引き起こす原因となる場合があった。
前記湿気硬化性ポリウレタンホットメルト樹脂(A)は、ポリオールとポリイソシアネートとを反応させて得られるものであり、「湿気硬化性」と「ホットメルト性」の2つの特性を具備するものである。
また、前記一般式[1]で示される化合物が有する加水分解性アルコキシシリル基としては、例えば、ハロシリル基、アルコキシシリル基、アシロキシシリル基、フェノキシシリル基、イミノオキシシリル基またはアルケニルオキシシリル基などの、加水分解され易いシリル基を使用することができる。
以下に、前記粒子状物質(b1)として代表的な顔料、難燃剤、充填剤、発泡剤についてより具体的に説明する。
また、無溶剤の混合システムを考慮した場合、本発明の混合方法によって得られた樹脂組成物(C)の吐出後のクリーニングシャフトによる押出洗浄機溝を有している装置がより好ましい。一般的に、低圧注入機の場合、高速ミキシングヘッドを有しており、作業終了後に溶剤などでミキシングヘッドを洗浄するか、ミキシングヘッド交換をする必要があり、洗浄工程に時間を費やしているが、かかる装置を使用した場合に、短時間での均一混合が可能となり、かつ洗浄に要する時間を画期的に短縮する事ができる。
各湿気硬化性ポリウレタンホットメルト樹脂の溶融粘度(mPa・s)は、コーンプレート粘度計(ICI社製)を用いて、測定温度125℃にて測定した。
実施例及び比較例で得た着色された各樹脂組成物を透明な容器に塊状で採取して、着色均一性を目視で観察して、下記の4段階で評価した。
◎:着色状態がきわめて良好である。
○:着色状態が良好である。
△:着色状態に若干色むらが認められる。
×:着色状態に色むらが認められる。
実施例及び比較例で得た着色された各樹脂組成物を、120℃に設定したロールコーターにて、厚み100μmのPETフィルム上に200μmで塗布して、その着色均一性を目視で観察して、下記の4段階で評価した。
◎:着色状態がきわめて良好である。
○:着色状態が良好である。
△:着色状態に若干色むらが認められる。
×:着色状態に色むらが認められる。
表1の配合に従い、1リットル4ツ口フラスコに、数平均分子量(Mn)が2000のポリテトラメチレングリコール(表1では「PTMG 2000」と省略。)の70質量部、及び、アジピン酸(表1では「AA」と省略。)とヘキサンジオールとを反応させて得られた数平均分子量(Mn)2000のポリエステルポリオール(表1では「HG/AA 2000」と省略。)の30質量部を加えて、120℃にて減圧加熱することにより水分が0.05質量%となるまで脱水した。次いで、それらを60℃に冷却した後、キシリレンジイソシアネート(表1では「XDI」と省略。)を15質量部、及び触媒としてジ−n−ブチル錫ジラウレート(表1では「DBTDL」と省略。)を0.01質量部加えた後、110℃まで昇温して、イソシアネート基含有量が一定となるまで5時間反応することにより樹脂組成物(A−1)を得た。前記樹脂組成物(A−1)の125℃における溶融粘度は4000mPa・sであり、イソシアネート基含有量は2.1質量%であった。
粒子状物質として温度60℃で1日乾燥することにより脱水したカーボンブラックを使用し、ビヒクルとして数平均分子量3000のグリセリンベースの3官能プロピレンオキサイド付加体を使用した。これらを[粒子状物質/ビヒクル]=30/70質量比の割合で仕込み、卓上ボールミルを用いて60℃で1000rpmの条件で30分間、均一になるまで混合攪拌することにより組成物(B−1)を調製した。
粒子状物質として温度60℃で1日乾燥することにより脱水した酸化チタン系白顔料を使用し、ビヒクルとして数平均分子量3000のグリセリンベースの3官能プロピレンオキサイド付加体を使用した。これらを[粒子状物質/ビヒクル]=60/40質量比の割合で仕込み、卓上ボールミルを用いて60℃で1000rpmの条件で30分間、均一になるまで混合攪拌することにより組成物(B−2)を調製した。
前記組成物(B−1)と組成物(B−2)を、[(B−1)/(B−2)]=10/90質量比の混合割合で仕込み、それらを、卓上ボールミルを用いて60℃で1000rpmの条件で30分間、均一になるまで混合攪拌することによって組成物(B−3)を調製した。
《樹脂組成物(C−1)、及び積層体シート1の製造》
120℃で加熱溶融した湿気硬化性ポリウレタンホットメルト樹脂(A−1)と、60℃に加温された前記組成物(B−3)とを、[(A−1)/(B−3)]=100/30質量比の混合割合となるように、MX型高圧ミキシングヘッド注入機(丸加化工機株式会社製。加温タンク、ホース及びヘッドの温度:120℃。各噴射ノズルの吐出圧力:1.5×104kPa)を用いてそれらを衝突混合することによって、樹脂組成物(C−1)を得た。前記樹脂組成物(C−1)を透明な容器に採取して、目視にて均一着色性を評価したところ、色ムラが全く無く、着色状態はきわめて良好であった。
また、加熱溶融状態の前記樹脂組成物(C−1)を、120℃に設定されたロールコーターを用いて、厚み100μmのPETフィルム上に、200μmのシート状に塗布し、硬化させることによって積層体シート1を得た。前記積層体シート1の均一着色性を目視にて評価したところ、色ムラが全く無く、着色状態はきわめて良好であった。
《樹脂組成物(D)、及び積層体シート2の製造》
120℃で加熱溶融した湿気硬化性ポリウレタンホットメルト樹脂(A−1)と、60℃に加温された前記組成物(B−3)とを、[(A−1)/(B−3)]=100/30質量比の混合割合となるように、低圧2液混合攪拌機(加温タンク、ホース及びヘッドの温度:120℃。各ノズルの吐出圧力:0.03×104kPa)を用いてそれらを衝突混合することによって、樹脂組成物(D)を得た。
前記樹脂組成物(D)を透明な容器に採取して、目視にて均一着色性を評価したところ、若干色ムラがあり、着色状態としてはあまり良くなかった。
また、加熱溶融状態の前記樹脂組成物(C−1)を、120℃に設定されたロールコーターを用いて、厚み100μmのPETフィルム上に、200μmのシート状に塗布し、硬化させることによって積層体シート2を得た。前記積層体シート2の均一着色性を目視にて評価したところ、部分的に色ムラが有り、着色状態としてはあまり良くなかった。
PTMG;ポリテトラメチレングリコール
HG ;1,6−ヘキサンジオール
AA ;アジピン酸
XDI ;キシリレン−ジイソシアネート
DBTDL;ジ−n−ブチル錫ジラウレート
Claims (10)
- 7.5×103kPa〜2.3×104kPaで加圧することによって噴射された加熱溶融状態の湿気硬化性ポリウレタンホットメルト樹脂(A)〔但し、前記樹脂(A)のコーンプレート粘度計を用いて125℃で測定した溶融粘度は、100〜10,000mPa・sの範囲である。〕と、7.5×103kPa〜2.3×104kPaで加圧することによって噴射された粒子状物質(b1)及び常温で液状または加熱溶融状態のビヒクル(b2)を含む組成物(B)とを衝突させることによってそれらを混合する方法。
- 前記湿気硬化性ポリウレタンホットメルト樹脂(A)と前記組成物(B)とをそれぞれ噴射する噴射ノズル開口部の開口率が5〜95%の範囲である、請求項1に記載の混合方法。
- 前記加熱溶融状態の湿気硬化性ポリウレタンホットメルト樹脂(A)の温度が80℃〜140℃の範囲である、請求項1に記載の混合方法。
- 前記組成物(B)の温度が30℃〜140℃の範囲である、請求項1に記載の混合方法。
- 前記湿気硬化性ポリウレタンホットメルト樹脂(A)が、末端にイソシアネート基を有するポリウレタンホットメルト樹脂、及び、末端にイソシアネート基と加水分解性シリル基とを有するポリウレタンホットメルト樹脂からなる群より選ばれる少なくとも1種である、請求項1に記載の混合方法。
- 前記湿気硬化性ポリウレタンホットメルト樹脂(A)のイソシアネート基含有率が、前記湿気硬化性ポリウレタンホットメルト樹脂(A)全量に対して0.5〜8.0質量%である、請求項1に記載の混合方法。
- 前記粒子状物質(b1)が、顔料、難燃剤、充填剤、及び発泡剤からなる群より選ばれる少なくとも1種である、請求項1に記載の混合方法。
- 前記ビヒクル(b2)がポリオールである、請求項1に記載の混合方法。
- 請求項1〜8のいずれかに記載の混合方法によって、前記加熱溶融状態の湿気硬化性ポリウレタンホットメルト樹脂(A)、粒子状物質(b1)、及び常温で液状または加熱溶融状態のビヒクル(b2)を含んでなる樹脂組成物(C)を製造する方法。
- 請求項1〜8のいずれかに記載の混合方法によって、加熱溶融状態の湿気硬化性ポリウレタンホットメルト樹脂(A)、粒子状物質(b1)、及び常温で液状または加熱溶融状態のビヒクル(b2)を含んでなる樹脂組成物(C)を製造し、加熱溶融状態の前記樹脂組成物(C)を基材上に塗布し、次いで硬化させることによって前記基材上に被膜を形成させることを特徴とする積層体の製造方法。
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