JP6873122B2 - 撥性表面を含むスプレー塗布システム構成要素及び方法 - Google Patents
撥性表面を含むスプレー塗布システム構成要素及び方法 Download PDFInfo
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- JP6873122B2 JP6873122B2 JP2018521616A JP2018521616A JP6873122B2 JP 6873122 B2 JP6873122 B2 JP 6873122B2 JP 2018521616 A JP2018521616 A JP 2018521616A JP 2018521616 A JP2018521616 A JP 2018521616A JP 6873122 B2 JP6873122 B2 JP 6873122B2
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- HTYPUNPKBFMFFO-UHFFFAOYSA-N platinum silver Chemical compound [Ag][Pt][Pt] HTYPUNPKBFMFFO-UHFFFAOYSA-N 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920013639 polyalphaolefin Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001748 polybutylene Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 229920002959 polymer blend Polymers 0.000 description 1
- 229920005594 polymer fiber Polymers 0.000 description 1
- 229920006254 polymer film Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001843 polymethylhydrosiloxane Polymers 0.000 description 1
- 229920005606 polypropylene copolymer Polymers 0.000 description 1
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- XAEFZNCEHLXOMS-UHFFFAOYSA-M potassium benzoate Chemical compound [K+].[O-]C(=O)C1=CC=CC=C1 XAEFZNCEHLXOMS-UHFFFAOYSA-M 0.000 description 1
- XRVCFZPJAHWYTB-UHFFFAOYSA-N prenderol Chemical compound CCC(CC)(CO)CO XRVCFZPJAHWYTB-UHFFFAOYSA-N 0.000 description 1
- 229950006800 prenderol Drugs 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- LLHKCFNBLRBOGN-UHFFFAOYSA-N propylene glycol methyl ether acetate Chemical compound COCC(C)OC(C)=O LLHKCFNBLRBOGN-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 239000011541 reaction mixture Substances 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
- 238000002390 rotary evaporation Methods 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 235000003441 saturated fatty acids Nutrition 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 150000004760 silicates Chemical class 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 238000000935 solvent evaporation Methods 0.000 description 1
- 238000009987 spinning Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 230000003068 static effect Effects 0.000 description 1
- 239000008117 stearic acid Substances 0.000 description 1
- 150000003457 sulfones Chemical class 0.000 description 1
- 230000003746 surface roughness Effects 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- QZZGJDVWLFXDLK-UHFFFAOYSA-N tetracosanoic acid Chemical compound CCCCCCCCCCCCCCCCCCCCCCCC(O)=O QZZGJDVWLFXDLK-UHFFFAOYSA-N 0.000 description 1
- TUNFSRHWOTWDNC-HKGQFRNVSA-N tetradecanoic acid Chemical compound CCCCCCCCCCCCC[14C](O)=O TUNFSRHWOTWDNC-HKGQFRNVSA-N 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 description 1
- RUELTTOHQODFPA-UHFFFAOYSA-N toluene 2,6-diisocyanate Chemical compound CC1=C(N=C=O)C=CC=C1N=C=O RUELTTOHQODFPA-UHFFFAOYSA-N 0.000 description 1
- KJIOQYGWTQBHNH-UHFFFAOYSA-N undecanol Chemical compound CCCCCCCCCCCO KJIOQYGWTQBHNH-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- AVWRKZWQTYIKIY-UHFFFAOYSA-N urea-1-carboxylic acid Chemical compound NC(=O)NC(O)=O AVWRKZWQTYIKIY-UHFFFAOYSA-N 0.000 description 1
- 238000007666 vacuum forming Methods 0.000 description 1
- 238000007740 vapor deposition Methods 0.000 description 1
- PXXNTAGJWPJAGM-UHFFFAOYSA-N vertaline Natural products C1C2C=3C=C(OC)C(OC)=CC=3OC(C=C3)=CC=C3CCC(=O)OC1CC1N2CCCC1 PXXNTAGJWPJAGM-UHFFFAOYSA-N 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 229920002554 vinyl polymer Polymers 0.000 description 1
- 238000001429 visible spectrum Methods 0.000 description 1
- 238000011179 visual inspection Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Images
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
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- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/24—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas with means, e.g. a container, for supplying liquid or other fluent material to a discharge device
- B05B7/2402—Apparatus to be carried on or by a person, e.g. by hand; Apparatus comprising containers fixed to the discharge device
- B05B7/2478—Gun with a container which, in normal use, is located above the gun
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- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/24—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas with means, e.g. a container, for supplying liquid or other fluent material to a discharge device
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- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05B—SPRAYING APPARATUS; ATOMISING APPARATUS; NOZZLES
- B05B7/00—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas
- B05B7/24—Spraying apparatus for discharge of liquids or other fluent materials from two or more sources, e.g. of liquid and air, of powder and gas with means, e.g. a container, for supplying liquid or other fluent material to a discharge device
- B05B7/2402—Apparatus to be carried on or by a person, e.g. by hand; Apparatus comprising containers fixed to the discharge device
- B05B7/2481—Apparatus to be carried on or by a person, e.g. by hand; Apparatus comprising containers fixed to the discharge device with a flexible container for liquid or other fluent material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
- B05D5/08—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
- B05D5/083—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Description
Rf−[Q−[C(R1)2−Si(R2)3−x(R3)x]y]z
(I)
式(I)において、基Rfは、ペルフルオロエーテル、ペルフルオロポリエーテル、又はペルフルオロアルカンのz価の基(すなわち、Rfは、(a)ペルフルオロエーテルの一価若しくは二価の基、(b)ペルフルオロポリエーテルの一価若しくは二価の基、又は(c)ペルフルオロアルカンの一価若しくは二価の基)である。基Qは、単結合、二価結合基、又は三価結合基である。各基R1は、独立して、水素又はアルキルである。各基R2は、独立して、ヒドロキシル基又は加水分解性基である。各基R3は、独立して、非加水分解性基である。変数xは、0、1、又は2に等しい整数である。変数yは、1又は2に等しい整数である。変数zは、1又は2に等しい整数である。
Rf−Q−[C(R1)2−Si(R2)3−x(R3)x]y
(Ia)
このような化合物は、式−Q−[C(R1)2−Si(R2)3−x(R3)x]yの単一の末端基が存在するため、単足性フッ素化シランと呼ぶことができる。変数yが1に等しい場合、単一のシリル基が存在し得、又は変数yが2に等しい場合、2つのシリル基が存在し得る。
Rf−[Q−[C(R1)2−Si(R2)3−x(R3)x]y]2
(Ib)
このような化合物は、式−Q−[C(R1)−Si(R2)3−x(R3)x]yの2つの末端基が存在するため、二脚性フッ素化シラン(bipodal fluorinated silane)と呼ぶことができる。各末端基は、変数yが1に等しい場合、単一のシリル基を有することができ、又は変数yが2に等しい場合、2つのシリル基を有することができる。式(Ib)は、Rf基の二価の性質を強調する以下の同等の式として書くことができる。
[(R3)x(R2)3−xSi−C(R1)2]y−Q−Rf−Q−[C(R1)2−Si(R2)3−x(R3)x]y
Rf−C(R1)2−Si(R2)3−x(R3)x
(Ia−1)
同様に、二価のRf基を有する式(Ib)の化合物において、Qが単一の共有結合であり、yが1に等しい場合、化合物は、式(Ib−1)のものである。
Rf−[C(R1)2−Si(R2)3−x(R3)x]2
(Ib−1)
Rf−Q−C(R1)2−Si(R2)3−x(R3)x
(Ia−2)
同様に、二価のRf基を有する式(Ib)の化合物において、Qが二価の基であり、yが1に等しい場合、化合物は、式(Ib−2)のものである。
Rf−[Q−C(R1)2−Si(R2)3−x(R3)x]2
(Ib−2)
−C(R1)2−Si(R2)3−x(R3)x
Rf−Q−[C(R1)2−Si(R2)3−x(R3)x]2
(Ia−3)
同様に、二価のRf基を有する式(Ib)の化合物において、Qが三価の基であり、yが2に等しい場合、化合物は、式(Ib−3)のものである。
Rf−[Q−[C(R1)2−Si(R2)3−x(R3)x]2]2
(Ib−3)
Rf−[(CO)N(R4)−CH2)k−CH2−Si(R2)3]2のより具体的な例は、式
R1L[Si(R2)3−x(R3)x]y
(II)
式(II)において、基R1は脂肪族又は芳香族炭化水素基である。Lは、共有結合又は二価の有機結合基、例えば、ウレタン基である。各R2は、独立して、ヒドロキシル基又は加水分解性基である。各R3は、独立して、非加水分解性基である。各変数xは、0、1、又は2に等しい整数である。変数yは、1又は2に等しい整数である。
R1LSi(R2)3−x(R3)x
(IIa)
(R3)x(R2)3−xSiLR1LSi(R2)3−x(R3)x
(IIb)
好適な二価基として、アルキレン、アリーレン、又はこれらの組み合わせが挙げられる。
R1[Si(R2)3−x(R3)x]y
(III)
式中、R1及びR3は、独立して、非加水分解性基であり、R2はヒドロキシルであり、xは2であり、yは1である。典型的な実施形態では、R1及びR3は、独立して、水素、C1〜C4アルキル(例えば、メチル、エチル)又はフェニルである。
(Rf−L−P)nA
[Rfはフッ素化基であり、
Lは、独立して、有機二価結合基であり、
Pは、独立して、カテナリーの二価ヘテロ原子含有カルボニル部分であり、
Aは、炭化水素部分であり、
nは、典型的には、1〜3の範囲である]によって表される化合物又は化合物の混合物を含む。
−SO2N(R’)(CH2)k−
−CON(R’)(CH2)k−
−(CH2)k−
−(CH2)kO(CH2)k−
−(CH2)kS(CH2)k−
−(CH2)kSO2(CH2)k−
−(CH2)kOC(O)NH−
−(CH2)SO2N(R’)(CH2)k−
−(CH2)kNR’−
−(CH2)kNR’C(O)NH−
C4F9SO2N(CH3)(CH2)kOC(O)−A−C(O)O(CH2)kN(CH3)SO2C4F9 (IVa)
又は、
C4F9SO2N(CH3)(CH2)kOC(O)−A (IVb)
[式中、k及びAは、既に記載したとおりである]のうちの1つを有する。
RfQO−[C(O)R1C(O)OR2O]n[C(O)R1C(O)]m−OQRf (V)
(RfQO−がフッ素化アルコールから誘導され、−OR2O−がフッ素化ポリオールから誘導され、−C(O)R1C(O)−がジカルボン酸から誘導される場合)、
RfQC(O)−[OR2OC(O)R1C(O)]n[OR2O]m−(O)CQRf (VI)
(RfQC(O)−がフッ素化酸から誘導され、−C(O)R1C(O)−がジカルボン酸から誘導され、−OR2O−がフッ素化ポリオールから誘導される場合)で表されてもよく、
式V〜VIのそれぞれにおいて、
nは、数字1、2、3、4、5、6、7、8、9、又は10から選択される数字又は範囲であり、
mは1であり、
Rfは、上記のように、フッ素化基であり、
Qは二価結合基であり、
R1は、多価(例えば、二価)炭化水素部分であり、
R2は、ペルフルオロアルキル基、ペルフルオロヘテロアルキル基、又はこれらの混合物等の側鎖フッ素化基Rfを有する二価の有機基である。
Rf−Q’ (VII)
[式中、
Rfは、フッ素化基、好ましくは上記のようなフルオロアルキル又は(例えば、C4)ペルフルオロアルキル基であり、
Q’は、(ポリアシル化合物の)末端アシル基又は(ポリオールの)ヒドロキシル基に対して反応性がある官能基を含む部分である]が挙げられる。
RfQO−C(O)NHR1NHC(O)−OQRf (VIII)
(RfQO−がフッ素化アルコールから誘導され、−C(O)NHR1NHC(O)−がジイソシアネートから誘導される場合)、又は
RfQO−[C(O)NHR1NHC(O)OR2O]n[C(O)NHR1NHC(O)]m−OQRf (IX)
(RfQO−がフッ素化アルコールから誘導され、−OR2O−がフッ素化ポリオールから誘導され、−C(O)NHR1NHC(O)−がジイソシアネートから誘導される場合)によって表されてもよく、
式VIII及びIXにおいて、
nは、数字1、2、3、4、5、6、7、8、9、又は10から選択される数字又は範囲であり、
mは1であり、
Rfは、上記のように、フッ素化基であり、
Qは、上記のような二価結合基であり、
R1及びR2は、上記のとおりである。
RfQO−[C(O)NHZR2ZNHC(O)OR1O]n[C(O)NHZR2ZNHC(O)]m−OQRf (X)
[式中、n、m、Rf、R1、及びR2は上記と同じであり、
−C(O)NHZR2ZNHC(O)−は、鎖延長したフッ素含有ポリオールの残基であり、Zは、C4〜C6炭化水素(例えばアルキレン)等のジイソシアネートの残基である]を有する。
Rf−Q” (XI)
[式中、
Rfは、フッ素化基、好ましくは上記のような(例えば、C4)ペルフルオロアルキル基のフルオロアルキルであり、
Q”は、末端イソシアネート基又はヒドロキシル基に対して反応性がある官能基を含む部分である]のものが挙げられる。
(Rf−L−P)nA
[Rfは、フッ素化基であり、
Lは、独立して有機二価結合基であり、
Pは、カテナリーの二価ヘテロ原子含有カルボニル部分、例えば、−C(O)O−であり、
Aは、炭化水素部分であり、
nは、典型的には1〜3の範囲である]を有する化合物である、実施形態3の構成要素である。
液体収容容器及び/又はライナー用の蓋と、含むスプレー塗布システムであって、少なくとも上記液体収容容器及び/又はライナーは、多孔質層及びその多孔質層の孔に浸透した潤滑剤を含む撥液性表面層又は実施形態1〜24による撥液性表面を備える、スプレー塗布システムである。
a)固体撥液性材料と非フッ素化有機ポリマーバインダーとを含み、撥液性表面はテーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性であり、
b)固体シリコーン撥液性材料を含み、又は
c)少なくとも1500g/モルのMn及び50,000g/モル以下のMn若しくは200℃以下の融解温度を有する固体フルオロケミカル撥液性材料
を含む、構成要素である。
撥液性表面は、
a)固体撥液性材料と非フッ素化有機ポリマーバインダーとを含み、撥液性表面はテーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性であり、
b)固体シリコーン撥液性材料を含み、又は
c)少なくとも1500g/モルのMn及び50,000g/モル以下のMn若しくは200℃以下の融解温度を有する固体フルオロケミカル撥液性材料
を含む、構成要素である。
撥液性表面は、
a)固体撥液性材料と非フッ素化有機ポリマーバインダーとを含み、撥液性表面はテーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性であり、
b)固体シリコーン撥液性材料を含み、又は
c)少なくとも1500g/モルのMn及び50,000g/モル以下のMn若しくは200℃以下の融解温度を有する固体フルオロケミカル撥液性材料
を含む、構成要素である。
撥液性表面は、
a)固体撥液性材料と非フッ素化有機ポリマーバインダーとを含み、撥液性表面はテーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性であり、
b)固体シリコーン撥液性材料を含み、又は
c)少なくとも1500g/モルのMn及び50,000g/モル以下のMn若しくは200℃以下の融解温度を有する固体フルオロケミカル撥液性材料
を含む、構成要素である。
IRデータは、Nicolet6700シリーズFT−IR分光計(Thermo Scientific(Waltham,MA))を使用して得た。
水接触角は、Rame−Hartゴニオメータ−(Rame−Hart Instrument Co.(Succasunna,NJ))を使用して測定した。前進角(θadv)及び後退角(θrec)は、シリンジを用いて水を、静止液滴へ、又は静止液滴から、供給して測定した(液滴体積約5μL)。測定は、各表面上の2つの異なる点で行い、報告する測定値は、各試料について4つの値の平均である(各液滴について、左側及び右側の測定値)。
試験表面をPPG Envirobase塗料に浸漬し、一晩静置した。次いで、試験基材を塗料から取り出し、5分間垂直に保持して、コーティングから塗料が潜在的に流れ落ちるようにした。その後も塗料によって被覆されている表面の割合(百分率で表示)を、目視検査によって推測した。
HFPOシランは、式F(CF(CF3)CF2O)aCF(CF3)−CONH(CH2)3Si(OCH3)3[式中、変数aは4〜20の範囲である]の化合物である。この材料は、HFPO−COOCH3(20g、0.01579モル)及びNH2CH2CH2CH2−Si(OCH3)3(2.82g、0.01579モル)を、N2 雰囲気下で、電磁撹拌棒、窒素(N2)入口、及び還流冷却器を備えた100mL3つ口丸底フラスコに仕込むことによって調製した。反応混合物を75℃で12時間加熱した。反応を赤外(IR)分光法によって監視し、エステルピークが消失した後、得られた透明で粘稠な油状物を更に8時間真空下で保持し、そのまま使用した。
α,ωHFPOジメチルエステルCH3OC(O)−HFPO−C(O)OCH3は、米国特許第7,718,264号の調製第26番に類似した方法によって調製した。
出発ジオールHFPO−CONHCH[CH2OH]2は、撹拌棒を備えた500mLの丸底に、100g(0.0704モル、1420MW)のHFPO−C(O)OCH3及び8.34g(0.0915モル)の2−アミノ−1,3−プロパンジオールを仕込み、75℃で2時間加熱することによって調製した。この反応に200gのメチル−t−ブチルエーテルを加え、黄色の油(おそらく未反応の2−アミノ−1,3−プロパンジオール)が反応から分離された。次いで、黄色の油は加えずに、反応を分液漏斗に注いだ。反応を20mLの2N HCl水溶液で洗浄し、一晩放置して分離させた。有機層を20mLの1N水酸化アンモニウムで洗浄し、30分放置して分離させ、20mLの水で洗浄し、30分放置して分離させ、無水硫酸マグネシウムで乾燥し、濾過し、最大95℃で約1.5時間濃縮して、ジオールHFPO−CONHCH[CH2OH]2を得た。
撹拌棒を備えた25mLジャーに、10g(570MW、285MW、0.0351当量)のPripol 2033、7.20g(205.29MW、0.0351モル)のGeniosil GF−40、及びDBTDLの10%MEK溶液100マイクロリットルを仕込んだ。このジャーをシールし、75℃の浴中に置き、磁気撹拌しながら2時間加熱した。2時間の終了時点で、反応のFTIR分析は、約2265cm−1に残留−NCOのピークを示さなかった。
PE1コーティング配合物の調製は、最初にNALCO 1115の分散体を、適量の蒸留(DI)水を添加することによって固形分5重量%まで希釈した。次いで、1M HNO3触媒を上記の希釈分散体に添加し、分散体のpHを2に調節した。
EX24〜EX66の試料は、種々の潤滑剤を、上記の表面処理された多孔質PE1〜PE23試料に浸透させることによって調製した。これは、潤滑剤が広がって表面処理された多孔質層の全体が覆われるまで、所望の潤滑剤をPE1〜PE23試料上に滴下し、その後、試料を垂直に一晩保持して、余分な潤滑剤が流れ去るようにすることで実施した。
熱成形低密度ポリエチレン(LDPE)PPS(商標)ライナー(400mL)は、3M製であった。
上記の撥性内表面を有するライナー及び撥性内表面のない同じライナーである比較ライナー(CE.F)をそれぞれ秤量した。70gのPPG Envirobase自動車用塗料を、撥性内表面を有するライナー及び撥性内表面のない同じライナーである比較ライナー(CE.F)内に注いだ。ライナーを手で振盪及び回転し、塗料が容器の側壁の全てに確実に触れるようにした。次いで、塗料をライナーから注ぎ出し、ライナーを逆さまにして5分間(撥性内面を有するライナー)又は約3時間(CE.F)置き、更に多くの塗料を排出させた。ライナーをそれぞれ再秤量し、残留塗料の質量を計算した。試験結果は以下のとおりであった。
材料
下記の実施例で使用した全てのフルオロケミカル化合物、非フッ素化バインダー及びフルオロポリマーは、25℃及び40°F(4.44℃)〜130°F(54.4℃)の範囲の温度で固体である。
MEFBSE(C4F9SO2N(CH3)C2H4OH)(357当量を有するフルオロケミカルアルコール)は、本質的に米国特許第2,803,656号(Ahlbrecht,et al.)の実施例1に記載の手順を用いて、ペルフルオロブタンスルホニルフルオリド(PBSF)をメチルアミンと反応させてMEFBSA(C4F9SO2N(CH3)H)を生成した後、エチレンクロロヒドリンと反応させることによって2段階で生成した。
フルオロケミカル2は、長鎖炭化水素酸(Unicide 350、C25平均)、及びMEFBSE(C4F9SO2N(CH3)C2H4OH)をフルオロケミカル1の合成と同じ方法でエステル化することによって生成した。
1滴の(例えば、PPG Envirobase)塗料(約0.2mL)を、試料(7.5cm×5.0cmのコーティングされたスライドガラス)の(例えば、撥性表面の)中央部分に21℃で塗布した。試料(例えば、スライドガラス)を直ちに垂直に方向付けた。塗料の液滴がスライドガラスを滑り落ちた場合は「合格」、そうでない場合は「不合格」と表記した。
試料の非撥性表面全体(すなわち、7.5cm×5.0cmのスライドガラスのコーティングされていない側)を、3M Companyから商品名「SCOTCH−BLUE PAINTERS TAPE」で入手したテープでマスキングした。次いで、試料(スライドガラス)を、21℃にて、(例えば、PPG Envirobase)塗料に3.5cmの深さまで10分間浸漬した(換言すれば、コーティングした表面の約半分を浸漬した)。試料(スライドガラス)を希釈塗料から取り出し、30秒間垂直に方向付け、マスキングテープを外した。次いで、浸漬したコーティングされた表面に残った塗料を目視で推測し、残留塗料被覆率の百分率で表した。
十分なサイズ(2.8×3.2cm)の試料を秤量した。試料の非撥性表面(すなわち、コーティングされていない側)全体を、テープ「SCOTCH−BLUE PAINTERS TAPE」でマスキングした。試料の撥性表面を、(例えば、PPG Envirobase)塗料に21℃にて10分間完全に浸漬した(例えば、30g)。次いで、試料を塗料から取り出し、マスキングテープを外し、試料をバインダークリップを用いて1分間垂直に方向付けた。試料の底縁をペーパータオルに接触させ、材料の底縁沿いに溜まっている可能性のある塗料を吸い取った。各試料の重量を再度測定し、面積当たりの残留塗料の量を計算した。コーティングされた表面に残った塗料を目視で推測し、残留塗料被覆率の百分率で表した。
ポリマーバインダー及びフッ素化添加剤を含有するPE32〜PE56コーティング溶液を調製し、下記の実施例(EX)及び比較例(CE)で使用した。
スライドガラス(7.5×5.0cm、厚さ0.1cm、Fisherより入手)をアセトンで洗浄し、WYPALLペーパータオルで拭いて乾燥させた。洗浄したスライドガラスを平坦な表面上に置き、約0.5mLの各コーティング組成物を、洗浄したスライドガラス上に、52番マイヤーロッドを用いて均一にコーティングし、21℃で約2時間乾燥した。これにより、最初は約133ミクロンで、溶媒蒸発後は5ミクロンのコーティングが得られる。
CE83は、その内壁にいかなるコーティング溶液も塗布せずに「そのまま」使用したLDPE PPSの400mL容器であった。
CE87は、「Earlex L0190”1 quart(946mL)PTFE Coated Metal Paint Container」(Home Depot USA Inc.(Atlanta,GA)から入手)の底から切り取った試料であった。この切り取り試料は、2.8cm×3.2cmの寸法の矩形であった。塗料撥性及び水接触角は、次のように評価された。
EX91は、ピペットでPE41溶液をライナー内に移し、溶液が容器の内部全体を濡らすまでライナーを回転することによってPPSライナーの表面をコーティングして調製した。次いで、コーティングした容器を回転して逆さまにし、余分なコーティング溶液を排出し、この逆さまの位置で室温にて2時間乾燥した。次いで、コーティングしたライナーの一部を側面から切り取り、塗料撥性試験に使用した。塗料撥性は、4種類の塗料で、試験方法6に従って評価した。
Spies Hecker:70体積%のWT389 Platinum Silver Permahyd Hi−TEC Base Coat 480と30体積%のHi−TEC WT6050
Glasurit:50体積%のJet Black 90−1250 Base Coatと50体積%の90 Adjusting Base 93−E3
Sikkens:70体積%のJet Black Autowave 391096と30体積%のAutowave WB 391196
CE92は、いかなる処理も行っていないPPSライナーの側面からの切断片であった。切断試料の寸法は、5cm×5cmであった。
シロキサン溶融添加剤(アルキルジメチコン)は、米国特許第9,187,678号の実施例14に記載のとおりに合成した。アルキルジメチコンを、190℃に保った25mm二軸押出機を用いて15重量%の負荷でNA217000 LDPE(Lyondell Basell(Houston,TX))に配合した。アルキルジメチコンを、加熱したギアポンプ及び移送ラインを用いて、120℃の液体として押出機に送った。このマスターバッチ溶融物を、撚合せダイを通じて冷却水浴中に押出し、13.6Kg/時の速度でペレット化した。
攪拌棒、加熱器、及びディーンスタークトラップを備えた丸底反応フラスコに、オクタデカン二酸(ODDA、30g、0.095モル)、FBSEE(27.5g、0.071モル)、MeFBSE(17.01g、0.048モル)、トルエン(100g)及びメタンスルホン酸(1g)を添加した。得られた混合物を115℃で15時間還流した。所望の量の水(3g)が回収されたら、温度を80℃に下げた。次いでK2CO3(2〜3g)を添加し、混合物を更に30分間撹拌した。FTIR分析は、ヒドロキシルピークが全く存在しないことを示した。混合物を熱濾過し、溶媒を回転蒸発により除去した。GPC及びポリスチレン標準を使用して分子量を測定し、Mn約2800g/モル及びMw約5400g/モルと決定された。
1つのフラスコ内で、Estane 5703(5g)をMEK(95g)に添加し、この混合物をEstaneが溶解するまで撹拌した。別のフラスコで、FC−3(5g)とMEK(95g)との混合物を撹拌し、フルオロケミカルが溶解するまで65℃に加熱した。上記の5重量%の溶液19gを高温(65℃)の5重量%のFC−3溶液1gと混合することによってコーティング溶液を調製した。
(Estane 5703/FC−3)コーティング溶液を、13番マイヤーロッド(RD Specialties)を用いてPETフィルム(3M Company)に適用した。コーティングされたPETフィルムを、21℃で少なくとも30分(EX101)又は110℃で10分間(EX102)のいずれかで乾燥した。
(Estane 5703/FC−3)コーティング溶液(約5mL)を、ピペットを用いてライナーの内側に適用した。ライナーを手で回転させて、コーティング配合物で完全に湿潤し、容器を逆さまにひっくり返すことで余分なコーティングを排出した。次いで、コーティングされたライナーを21℃で少なくとも2時間乾燥した。
十分なサイズ(例えば、6cm×2cm)の試料を調製し、テ−バー摩耗試験機(Taber Industries 5750線形摩耗試験機)に取り付けた。クロックメーター用摩擦布(Testfabrics,Inc.からのAATC Crockmeter Square)を、ゴムバンドで摩耗試験機のヘッドに取り付けた。摩耗試験機のヘッドの上に追加のおもりは置かなかった。サイクル速度を15サイクル/分に設定し、各基材に摩耗サイクルを2回施した(換言すれば、摩耗試験機のヘッドが2回前後した)。
Claims (15)
- 水との後退接触角が90度から135度である撥液性表面を備え、前記撥液性表面が、シラン又はシロキサン材料を含む表面層を備え、前記撥液性表面が、固体撥液性材料を含む、スプレー塗布システムの構成要素。
- 前記撥液性表面が、潤滑剤浸透面ではない、請求項1に記載の構成要素。
- 前記シロキサン材料が、シロキサン主鎖及び平均で少なくとも8個の炭素原子を有する炭化水素側鎖を含む、請求項1または2に記載の構成要素。
- 水との後退接触角が90度から135度である撥液性表面を備え、前記撥液性表面が、シラン又はシロキサン材料を含む表面層を備え、前記構成要素の少なくとも前記撥液性表面が、熱加工可能なポリマーとシロキサン材料溶融添加剤とを含む、スプレー塗布システムの構成要素。
- 前記撥液性表面が、テーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性である、請求項1〜4のいずれか一項に記載の構成要素。
- 水との後退接触角が90度から135度である撥液性表面を備え、前記撥液性表面が、1500〜50000g/モルのMnを有するフルオロケミカル材料を含む、スプレー塗布システムの構成要素。
- 前記フルオロケミカル材料が、200℃以下の融解温度を有する、請求項6に記載の構成要素。
- 前記撥液性表面が、平均で少なくとも8個の炭素原子を有する末端ペルフルオロアルキル基、側鎖ペルフルオロアルキル基、及び連続するアルキレン基を含むフルオロケミカル材料を含む、請求項6または7に記載の構成要素。
- 水との後退接触角が90°〜135°の範囲であって固体撥液性材料と非フッ素化有機ポリマーバインダーとを含む撥液性表面を備え、前記撥液性表面がテーバー線形摩耗試験機により摩耗サイクルを15サイクル/分で2回施した後に撥液性であり、前記固体撥液性材料が、シロキサン材料、1500〜50000g/モルのMnを有するフルオロケミカル材料、または200℃以下の融解温度を有するフルオロケミカル材料を含む、スプレー塗布システムの構成要素。
- 液体収容容器、液体収容容器用のライナー、液体収容容器若しくはライナー用の蓋、又はこれらの組み合わせである、請求項1〜9のいずれか一項に記載の構成要素。
- 熱可塑性ポリマー材料を含む、請求項1〜10のいずれか一項に記載の構成要素。
- 前記撥液性表面が、少なくとも10g/リットルの揮発性有機溶媒を有する水性塗料を撥き、前記揮発性有機溶媒が水溶性である、請求項1〜11のいずれか一項に記載の構成要素。
- 残留塗料の質量が0.01g/cm2以下である撥液性表面を備えるか、
撥液性表面の水との前進接触角と後退接触角と間の差が15又は10未満である撥液性表面を備えるか、
10重量%の2−n−ブトキシエタノールと90重量%の脱イオン水とを含有する溶液との後退接触角が少なくとも40°である撥液性表面を備えるか、
垂直に方向付けたときに塗料の液滴が表面から滑り落ちる撥液性表面を備える、
請求項1〜12のいずれか一項に記載の構成要素。 - スプレーガンと、
前記スプレーガンに取り付けられた液体収容容器と、
前記液体収容容器用の蓋と、
を含むスプレー塗布システムであって、少なくとも前記液体収容容器が請求項1〜13のいずれか一項に記載の構成要素である、スプレー塗布システム。 - スプレーガンと、
前記スプレーガンに取り付けられた液体収容容器と、
前記液体収容容器用のライナーと、
前記液体収容容器及び/又はライナー用の蓋と、
を含むスプレー塗布システムであって、少なくとも前記液体収容容器及び/又はライナーが請求項1〜13のいずれか一項に記載の構成要素である、スプレー塗布システム。
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US201662327783P | 2016-04-26 | 2016-04-26 | |
US62/327,783 | 2016-04-26 | ||
PCT/US2016/058166 WO2017074817A1 (en) | 2015-10-28 | 2016-10-21 | Spray application system components comprising a repellent surface & methods |
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AU2017255540B9 (en) | 2020-04-23 |
JP2019514796A (ja) | 2019-06-06 |
EP3368224A1 (en) | 2018-09-05 |
AU2016346920A1 (en) | 2018-05-10 |
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CA3003259A1 (en) | 2017-05-04 |
CA3022467A1 (en) | 2017-11-02 |
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CN109070129A (zh) | 2018-12-21 |
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AU2016346920B2 (en) | 2020-04-30 |
WO2017189684A1 (en) | 2017-11-02 |
EP3448579A1 (en) | 2019-03-06 |
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