CN1135769A - 脱膜剂、由该脱膜剂得到的硬化膜及使用该脱膜剂的成型方法 - Google Patents

脱膜剂、由该脱膜剂得到的硬化膜及使用该脱膜剂的成型方法 Download PDF

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CN1135769A
CN1135769A CN94194244A CN94194244A CN1135769A CN 1135769 A CN1135769 A CN 1135769A CN 94194244 A CN94194244 A CN 94194244A CN 94194244 A CN94194244 A CN 94194244A CN 1135769 A CN1135769 A CN 1135769A
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compound
carbonatoms
alkyl
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CN1053005C (zh
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山名雅之
细见朋浩
坂下浩敏
柏木正人
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Daikin Industries Ltd
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Abstract

本发明涉及一种脱膜剂，该脱膜剂是由式：[式中，R1表示上式]
(其中，R3、R4分别表示碳原子数1-4的烃基)R2表示碳原子数1-4的烃基或者卤代烃基，n是3或4]表示的含有硅的化合物和1分子内含有2个以上羟基或烷氧基的含有硅和/氟的化合物组成，本发明提供的脱膜剂脱膜性能优良、脱膜寿命长、成型品的表面成型性良好、对成型品的二次加工性无影响。

Description

脱膜剂、由该脱膜剂得到的硬化 膜及使用该脱膜剂的成形方法
本发明涉及脱膜剂、由该脱膜剂得到的硬化膜及使用该脱膜剂的成形方法，更详细地是有关在制造由合成树脂及橡胶等高分子化合物形成的成形品时使用的脱膜剂、硬化膜及成形方法。
为了得到由树脂和橡胶形成的成形品，要将树脂和橡胶材料充填在(金属)模具中进行成形。但通常在充填前要在模具上预先涂敷脱膜剂。
脱膜剂例如有石蜡、聚乙烯蜡等蜡类，聚二甲基硅氧烷油、硅树脂等聚硅氧烷类，乙二醇，脂肪酸衍生物，含有全氟代烷基化合物等有机化合物，或将矿物油，滑石粉，云母等无机化合物分散或者溶解在水或有机溶剂中使用。
这些脱膜剂通常是每次都要涂敷，涂敷以后才能使用。从工作效率方面考虑，为了减少工序数就希望开发一种脱膜寿命被延长的脱膜剂。而且，由于每次都要涂敷，所以就发生了由脱膜剂的堆积造成的模具污染问题，特别是蜡类脱膜剂造成的污染程度最严重。而且，因为每次都要涂敷，所以脱膜剂基本上有向成形品一侧的移动，这就影响了成形品的粘性，结果造成后序工序中向成形品涂覆不良或粘合不良等的原因。成形后，必需用三氯乙烷等有机溶剂洗涤。特别是硅酮类脱膜剂容易引起涂覆或粘合不良。
另外，由聚氨酯泡沫塑料制造成形品时，得到的成形品的表面产生一些网眼。特别是用硅酮油作脱膜剂时，这种现象非常显著。为了解决这些缺点，正在开发各种各样的脱膜剂。如碳原子数4-20的全氟代烷基磷酸酯或者它的盐及硅酮油的混合物(特公昭53-23270号、同53-23271号公报)、含有碳原子数4-20的全氟代烷基磷酸酯或者它的盐及硅漆的混合物(特公昭5748035号公报)、含有全氟代烷基的聚醚化合物及硅酮油等的混合物(特公昭59-32513号公报)等。这些都是脱膜性能优良的脱膜剂，脱膜寿命也比以前的脱膜剂长。而且，由含全氟代烷基的聚醚化合物和硅酮油等混合物组成的脱膜剂对大部分高分子化合物成形品的二次加工性几乎没影响。但是这些脱膜剂也不能满足随着高分子化合物成形品形状的复杂化和大型化对脱膜性能和脱膜寿命等的要求。
另外，作为形成硬化膜型的能延长脱膜寿命的脱膜剂，在特公平3-39804号公报中记载了含有全氟代烷基丙烯酸类聚合物和オルガノシルセスキオキサン梯形聚合物的脱膜剂。这些脱膜剂在初姆的脱膜性能优良，脱膜寿命也能在某种程度上被延长，但是因为硬化膜的强度不充分，所以不能得到满意的脱膜寿命。
在特公平3-11605号公报中，记载了含有聚二甲基硅氧烷和以式：
                   (Z1O)uSiZ24-u(式中、Z1代表甲基、乙基、丙基或者甲氧基乙基、Z2代表碳原子数1-4的一价烃基；u代表3或者4。)表示的烷氧基硅烷或者由它部分水解及缩合生成的低聚物生成物及四烷基钛酸酯等金属烷氧化物的脱膜剂。但是，这些脱膜剂的脱膜寿命和二次加工性都不充分。
本发明鉴于上述问题，目的在于获得脱膜性能优良、脱膜寿命长、成形品表面成形性良好、对成形品涂覆和粘合等二次加工性没有影响的脱膜剂。
本发明是关于用通式(I)：
         R1nSiR24-n    (I)〔式中，R1表示
Figure A9419424400091
(其中R3、R4分别表示碳原子数为1-4的烃基)R2表示碳原子数1-4的烃基或卤代烃基，n代表3或者4〕表示的含有硅的化合物(A)及，(B)1分子内有2个以上羟基或者烷氧基的含有硅和/或氟的化合物组成的脱膜剂、由该脱膜剂得到的硬化膜和使用该脱膜剂的成形方法。
本发明中所用的通式(I)：
           R1nSiR24-n    (I)所示的含硅化合物(A)中式R1表示以式
Figure A9419424400092
所示的基团，但从反应性、非腐蚀性、原料容易得到等方面考虑，是最优选的。共中R3、R4分别表示碳原子数1-4的烃基，具体为甲基、乙基、丙基、丁基、异丙基、异丁基、叔丁基等，但从反应性方面R3、R4考虑最好分别是甲基、乙基。作为R3和R4的组合，从反应性方面考虑，最好有一方是甲基或乙基。R2是碳原子数1-4的烃基或者卤代烃基。烃基有甲基、乙基、丙基、丁基、异丙基、异丁基、叔丁基等，卤代烃基有三氟丙基、三氯乙基等。从脱膜性和反应性方面考虑，优选碳原子数1-2的烃基。因为n是3或者4，所以R2是1个或者不存在。
上述通式(I)表示的化合物(A)有用通式(II)：
              R1nSiR24-n    (II)〔式中，R1表示(其中R3、R4分别表示碳原子数1-4的烃基)R2表示碳原子数1-4的烃基或者卤代烃基，n是3或者4〕表示的化合物。
作为含硅化合物(A)具体可以使用
Figure A9419424400103
Figure A9419424400111
等脱羧酸型、等脱酮型、
Figure A9419424400113
等脱酰胺型、
Figure A9419424400114
等脱胺型、
Figure A9419424400115
Figure A9419424400121
等脱肟型。
上述含硅化合物(A)有使如下说明的含硅和/或氟的化合物(B)交联的作用。
1分子内有2个以上羟基或者烷氧基的含硅和/或氟的化合物(B)如下所列：
如用通式(V)：
Figure A9419424400122
〔式中、j是正的整数、k是0或者正的整数、j+k的平均值是10以上，优选20-5000、X1、X2表示-OH、-OR12、-R13NH2、-R14OH、-R15COOH、-R15SH或者-R12、X3表示-OH、-OR12、-R13NH2、-R14OH、-R15COOH或者-R15SH(但当K是0时，X1、X2都是-OH或者-OR12，当K不是0时，X1、X2、X3至少有2个是-OH或者-OR12，R12表示碳原子数1-4的烷基、卤代烷基或者苯基，R13表示碳原子数1-10的亚烷基或R16NHCH2CH2-CR16表示碳原子数1-4的亚烷基)，R14表示
Figure A9419424400131
(其中，a是0或者1-15的整数， b是0或者1-15的整数，c是1-10的整数，d是1-5的整数)，R15表示碳原子数1-10的亚烷基)，R5、R6、R7、R8、R9、R10、R11表示碳原子数1-4的烷基、卤代烷基或者苯基〕。
另外，以无规则和/或嵌段结合。
R5、R6、R7、R8、R9、R10、R11、R12具体分别是甲基、乙基、丙基、异丙基、丁基、异丁基、叔丁基等烷基、三氟乙基、三氟丙基、三氯丙基等卤代烷基、苯基等。从反应性和脱膜性方面考虑优选甲基、乙基、三氟丙基等。
R13具体为-CH2-、CH22、CH23 、CH24、
Figure A9419424400141
等亚烷基、-CH2CH2NHCH2CH2-、-CH2CH2CH2NHCH2CH2-等，但从反应性和脱膜性方面考虑优选-(CH2)2-、-(CH2)3-、-(CH2)4-等。
R14具体为CH22、CH23  、CH24、CH210、-CH2CH2OCH2CH2CH2-、CH2CH2O15CH2CH2CH2-、
Figure A9419424400143
等，但从反应性和脱膜性方面考虑优选-(CH2)-、-(CH2)3-、-(CH2)4-、-CH2CH2OCH2CH2CH2-。
R15具体为CH22、CH23、-(CH24、CH25、CH210等，但从反应性和脱膜性方面考虑优选-(CH2)2-、-(CH2)3-、-(CH2)4-等。
X1、X2具体为-OH、-OCH3、-OCH2CH3、-OCH2CH3、-CH2CH2CH2NH2、-CH2CH2CH2OH、-CH2CH2CH2OCH2CH2OH、-(CH2)10-COOH、CH2CH2CH2SH、-CH3、-CH2CH3等，但从反应性、脱膜性方面考虑优选-OH、-OCH3、-OCH2CH3、-OCH2CH2CH3等。
X3具体为-OH、-OCH3、-OCH2CH3、-OCH2CH2CH3、-CH2CH2CH2NH2、-CH2CH2CH2OH、-CH2CH2CH2OCH2CH2OC、-(CH2)10-COOH、-CH2CH2CH2SH等，但从反应性、脱膜性方面考虑优选-OH、-OCH3、-OCH2CH3、-OCH2CH2CH3。
j从反应性、脱膜性方面考虑最好是10-5000的整数。
k从反应性、脱膜性方面考虑最好是0-500的整数。
用通式(V)表示的化合物，可以混合使用j和k的总数不同的物质，j和k的总数平均为10以上，从反应性和脱膜性方面考虑最好是20-5000的整数。
a从反应性、脱膜性方面考虑最好是0-15的整数。
b从反应性、脱膜性方面考虑最好是0-15的整数。
c从反应性、脱膜性方面考虑最好是1-10的整数。
用通式(V)表示的化合物具体有：
Figure A9419424400151
(P平均是20-5000)(P平均是20-5000)
Figure A9419424400162
(j+k平均是20-5000)
Figure A9419424400163
(j+k平均是20-5000)
Figure A9419424400164
(j+k平均是20-5000)
Figure A9419424400165
(j+k平均是20-5000)
Figure A9419424400171
(j+k平均是20-5000，k是2以上)(j+k平均是20-5000，k是2以上)(j+k平均是20-5000，k是2以上)
Figure A9419424400174
(P平均是20-5000)等。上述通式(V)表示的化合物中，优选用通式(VIII)：(式中、R5和R6分别表示碳原子数1-4的烷基或者卤代烃基或者苯基，X4、X5分别表示氢原子或者碳原子数1-4的烃基，m平均为10以上，优选20-5000)表示的化合物。
R5、R6具体为甲基、乙基、丙基、丁基、异丙基、异丁基、叔丁基等烷基、三氟乙基、三氟丙基、二氟乙基、三氯丙基等卤代烷基。从反应性和脱膜性方面考虑优选甲基、乙基、三氟乙基、三氟丙基等。
X4、X5具体地为H、CH3、CH2CH3、
Figure A9419424400181
其中，从反应性方面考虑优选H、CH3。
用通式(VIII)表示的化合物，可以混合使用m不同的物质，m平均为10以上，从反应性、脱膜性方面考虑优选20-5000，更优选20-3000，最优选20-2000。
用通式(VIII)表示的化合物具体为：(P平均20-5000)
Figure A9419424400183
(P平均是20-2000)(P平均是20-2000)(P平均是20-2000)
(P平均是20-2000)
还有用通式(VI)：
Y1OCH2R16O-R18-R17CH2OY2    (VI)〔式中，Y1、Y2分别表示氢原子或者碳原子数1-4的烃基，R16表示从-CF2、-CF2CF2-、
Figure A9419424400194
R17表示从-CF2-、-CF2CF2-、 R18表示从组成的组中选出的至少一种结构单元(R19表示
Figure A9419424400202
或-CF2CF2CF2-、S1+S2+S3平均是5以上，优选10-200)〕表示的化合物。
另外，上述R18可以是单独聚合物、无规共聚物、嵌段共聚物、或者交替共聚物中的任意一种。
Y1、Y2具体可以是氢原子、甲基、乙基、丙基、异丙基、丁基等。其中，从反应性方面考虑优选氢原子、甲基。
用通式(VI)表示的化合物，可以混合使用S1+S2+S3不同的物质，S1+S2+S3平均是5以上，从反应性方面考虑优选10-200，更优选10-100，最优选是10-50。
用通式(VI)表示的化合物优选如下所示的例子。HOCH2(CF2O)10(CF2CF2O)12CF2CH2OHHOCH2CF2CF2O(CF2CF2CF2O)10CF2CF2O(CF2CF2CF2O)10CF2CF2CH2OHCH3OCH2CF2CF2O(CF2CF2CF2O)20CF2CF2O(CF2CF2CF2O)20CF2CF2CH2OH还有用通式(VII)
Figure A9419424400211
(式中，Rf表示碳原子数6-21的全氟代烷基、A1是碳原子数2-6的亚烷基、A2是氢原子或者碳原子数1-4的烷基，A3是碳原子数1-4的烷基，S6是2或者3)表示的化合物。
Rf具体为：CF3(CF2)5、CF3(CF2)7、CF3(CF2)9、CF3(CF2)11、CF3(CF2)13、CF3(CF2)15、CF3(CF2)17、CF3(CF2)19、
Figure A9419424400212
其中，从脱膜性方面考虑优选CF3(CF2)7、CF3(CF2)9、CF3(CF2)11、CF3(CF2)1A1具体为：-CH2CH2-、-CH2CH2CH2CH2 、-(CH2)6-，但从脱膜性方面考虑优选-CH2CH2-。
A2具体为氢原子、 -CH3、-CH2CH3、-CH2CH2CH3、 -CH2CH2CH2CH3，但从反应性方面考虑优选氢原子、-CH3、-CH2CH3。
A3具体为甲基、乙基、丙基、丁基、异丙基、异丁基等，但从反应性方面考虑优选甲基或者乙基。
S6从反应性方面考虑优选是3。
另外，还有用20％(重量％，以下同样)以上的以通式(III)：
              RfA4A5(式中，Rf和上述相同，A4是碳原子数1-6的亚烷基，A5是
Figure A9419424400231
)表示的化合物和2％以上的用通式(IV)：
            A6OA7A8(式中，A6是氢原子或者碳原子数1-4的烃基，A7是碳原子数1-6的亚烷基，A8是)表示的化合物作为共聚合成分的数均分子量是1000以上的共聚物，但从脱膜性方面考虑优选数均分子量3000以上的。
Rf与上述相同。
A4具体为：-CH2-、-CH2CH2-、-CH2CH2CH2CH2-、
Figure A9419424400233
但从脱膜性方面考虑优选-CH2-、-CH2CH2-。用通式(III)表示的化合物具体为：CH2＝CHCO2CH2CH2(CF2)7CF3、CH2＝CHCO2(CH2)6(CF2)15CF3、CH2＝CHCO2CH2CH2(CF2)4CF3。
A6具体地为氢原子、甲基、乙基、丙基、丁基、异丙基、异丁基等。但从反应性方面考虑优选氢原子、甲基。
A7具体为：-CH2-、-CH2CH2-
Figure A9419424400243
-(CH2)6-。
用通式(IV)表示的化合物具体为CH2＝CHCO2CH2CH2OH、CH2＝CHCO2CH2CH2CH2OH、
Figure A9419424400244
CH2＝CHCO2CH2CH2OCH2CH3、CH2＝CHCO2CH2OCH2CH2CH2CH3。
用通式(III)表示的化合物在共聚物中含有20％以上，但从脱膜性方面考虑优选含有40％以上，更优选含有80％以上，优选上限是98％。如低于20％，则脱膜性能就有变坏的倾向。
用通式(IV)表示的化合物在共聚物中含有2％以上，但从反应性方面考虑优选含有3％以上，更优选含有5％以上，优选上限是20％。如低于2％，则反应性就有变坏的倾向。
上述共聚物的共聚合成分除用通式(III)、(IV)表示的化合物以外，也可以使用乙烯、丙烯、氯乙烯、偏氯乙烯、乙酸乙烯、乙烯正丁醚和甲基丙烯酸甲酯、丁基丙烯酸甲酯、十二烷基丙烯酸酯、十八烷基丙烯酸酯、2-乙基己基丙烯酸酯、环氧丙基丙烯酸甲酯等丙烯酸酯类，但从脱膜性方面考虑优选十二烷基丙烯酸酯、十八烷基丙烯酸酯、2-乙基己基丙烯酸酯等高级醇的丙烯酸酯类。
含有硅和/或氟的化合物(用通式(III)表示的化合物和用通式(IV)表示的化合物作为共聚合成分的共聚物，用通式(V)、通式(VI)、通式(VII)或者通式(VIII)表示的化合物)因为1分子内具有2个以上羟基或者烷氧基，所以进行交联反应以后能得到脱膜性优良的硬化膜。
含有硅和/或氟的化合物有如上述例举的6种化合物，这些化合物可以分别单独或者组合使用，将不同种类的化合物组合起来使用也可以。
本发明的脱膜剂中，脱膜性最好的是上述含有硅和/或氟的化合物(用通式(III)表示的化合物和用通式(IV)表示的化合物作为共聚合成分的共聚物，用通式(V)、通式(VI)、通式(VII)或者通式(VII)表示的化合物)。
本发明中的脱膜剂，除含有上述的含有硅的化合物(A)和含有硅及/或氟的化合物(B)以外，根据需要，也可加入硬化促进剂、溶剂等。
硬化促进剂可在含有硅的化合物和含有硅及/或氟的化合物不反应或者反应慢时，适当地添加。硬化促进剂有：四烷基钛酸盐、四烷基锗酸盐、四烷基锆酸盐、三烷氧基钒酸等金属醇盐类、辛酸锌、辛酸锡等有机酸盐类等。
溶剂可以用不含有羟基等的与上述含有硅的化合物(A)或者含有硅及/或氟的化合物(B)具有反应性的物质。优选脂肪族烃、脂环式烃、芳香族烃、卤代烃、硅氧烷类化合物。脂肪族类烃有己烷、庚烷、辛烷、癸烷、异辛烷等。脂环式烃有环己烷等。芳香族烃有甲苯、二甲苯、苯、乙苯等。卤代烃有三氯乙烷、三氯三氟乙烷、二氯甲烷、二氯一氟乙烷、全氯代乙烯、全氟代乙烷、HCFC141b等。硅氧烷类化合物有聚硅氧烷、环状多二甲基硅氧烷等。还可以用丙酮、丁酮、甲基异丁基甲酮等酮类化合物、乙酸乙酯、乙酸丁酯等酯类。
上述含有硅的化合物(A)和含有硅及/或氟的化合物(B)的重量比一般是1/99-80/20，优选2/98-40/60，最优选2/98-30/70。如低于1/99或高于80/20，则不能形成良好的交联膜，脱膜性有变坏的倾向。
硬化促进剂的量由含有硅的化合物(A)和含有硅及/或氟的化合物(B)的反应性决定，如：一般为含有硅的化合物(A)和含有硅及/或氟的化合物(B)的合计重量的0-10％，优选1-7％。如高于10％则脱膜性有变坏的倾向。
使用溶剂时，溶剂的量一般是使溶剂以外的成分的浓度为0、1-20％，优选0、5-10％；最优选1-10％。如该浓度低于0、1％，则难以形成良好的脱膜剂膜，如高于20％，则粘度过高，使涂覆变得困难。
本发明的脱膜剂，例如可将含有硅的化合物(A)及含有硅及/或氟的化合物(B)、及根据需要加入的溶剂、硬化促进剂及其它成分在常温下混合，得到一液型脱膜剂。含有硅的肟化合物与含有硅及/或氟的化合物的反应性高时，将硬化促进剂和其它成分的混合物分开保存，得到二液型脱膜剂也可以。
例如，本发明的一液型脱膜剂是在常温下，在金属模具的内侧刷涂或者喷雾涂覆，常温或者加热，即可形成本发明的硬化膜。加热温度因材料而异，一般在250℃以下，优选在20-200℃。如低于0℃，则硬化难以进行，如高于250℃，则脱膜剂成分容易发生分解。二液型脱膜剂是把硬化促进剂和其它成分在使用前混合，然后向模具内侧刷涂或者喷雾涂覆，如果需要可通过加热形成本发明的硬化膜。加热温度一般随材料不同而不同，通常在250℃以下，优选20-200℃。如低于0℃，则硬化难以进行，如高于250℃，则脱膜剂成分容易起分解反应。本发明硬化膜的膜厚没有特别限定，但不管是一液型、二液型，为了得到良好的脱膜性一般是0.1-100μm，优选0.2-20μm，最优选0.5-10μm。
本发明中脱膜剂的硬化过程，以脱肟型为例如下所示：(1)光进行脱肟反应，(2)然后通过进行脱水反应或脱醇反应而进行交联反应。
(1)脱肟反应
Figure A9419424400281
(2)脱水反应(交联反应)
Figure A9419424400282
或者，脱醇反应(交联反应)
Figure A9419424400283
(式中，HO-K1、R7O-K2(R7是碳原子数1-4的烃基)代表在上述1分子内有2个以上羟基或烷氧基的含有硅和/或氟的化合物)。
用本发明的脱膜剂实施以下成形方法。即把上述的含有硅的化合物(A)和含有硅及/或氟的化合物(B)用上述方法向模具内侧涂覆，根据上述的机理使之硬化，在模具内形成硬化膜，之后把成形用组合物充填在该模具内成形为成形品，将成形品从该模具中脱膜。
使用本发明的脱膜剂的模具是铝裂、SUS裂、铁裂、环氧树脂裂、木裂的模具等，或镍电铸或镀铬模具。
利用本发明的脱膜剂脱膜的成形品主要是使用以聚氨酯泡沫塑料、环氧树脂、酚醛树脂、FRP等热固性树脂、聚氨酯橡胶、H-NBR、NBR、硅橡胶、EPDM、CR、NR、氟橡胶、SBR、BR、IIR、IR等橡胶类等作为主体的成形用组合物得到的成形品。
本发明中的脱膜剂可以使用喷射剂充填在气雾剂罐中以后使用。喷射剂有脂肪族烃、卤代烃、二氧化碳、氮气等，脂肪族烃有丙烷、丁烷、LPG、二甲基醚等。卤代烃有R-11、R-12、HFC-134a、HCFC-142b、HCFC-22、HCFC-141b等。上述喷射剂在脱膜剂中一般含有10-95％，优选20-90％，最优选30-90％。如低于10％，则不能良好地喷射，不能形成均一的膜，如高于95％，则膜很薄，脱膜性有降低的倾向。
以下例举实施例和比较例进一步说明本发明，但本发明不仅仅局限在这些实施例。实施例1
混合含有硅的化合物CH3Si(ON＝C(CH3)2)32份(重量份，以下相同)、1分子内有2个以上羟基或者烷氧基的含有硅和/或氟的化合物93份交联促进剂四(2-乙基己基)钛酸盐5份和溶剂甲苯调制成本发明的脱膜剂。甲苯的量占脱膜剂中的95％，即其它3个成份的总量占5％。
对该脱膜剂进行以下的连续脱膜性实验、涂覆性实验和成形性实验。
〔连续脱膜性实验〕
(脱膜剂的脱膜性能和脱膜寿命)
将脱膜剂刷涂在内侧尺寸为6cmφ×1cm的铝制模具上，将模具在150℃加热10分钟以使脱膜剂硬化，在模具内侧形成硬化膜。硬化膜的膜厚是2.5μm。
将以下组成的聚氨酯组合物用搅拌器充分搅拌以后注入上述模具中。
＝FA9121)                               100份
乙二醇                                   19份
R-11(三氯-氟甲烷)                        5份
DABCO(1，4-二氮杂二环〔2，2，2〕辛烷)    0.9份
二丁基锡二月桂酸盐                       0.025份
ミリォネ-トMTL2)                        104份其中，1)是三洋化成工业(株)裂的多元醇，2)是日本聚氨酯工业(株)制的异氰酸酯。
使在室温硬化10分钟成形为聚氨酯成形体，用拉力实验和(拉力速度20mm/min)，牵拉予先竖在聚氨酯中的针，测定拉力(g/cm2)，根据以下标准评价脱膜性能，结果如表7所示。A  100g/cm2以下B  100g/cm2以上200g/cm2以下
C  200g/cm2以上300g/cm2以下
D  300g/cm2以上
然后，不再涂覆脱膜剂，把聚氨酯成形、脱膜的工序重复进行50次。评价第10次、第30次、第50次成形后的脱膜性能。结果如表7所示。〔涂覆性实验〕(成形品的二次加工性)
在连续脱膜性实验中第一次成形后的聚氨酯成形体中混合如下组成的底漆以后，进行刷涂。
      プラニツト  L#753)            100份
 プラニツトL#75シンナ-4)            100份其中，3)是大日本涂料(株)制的丙烯酸类涂料底漆，4)是该社制的稀料(thinner)。
在80℃燥10分钟后，将以下所示组成的涂料刷涂在底漆层上。
プラニツトS5)                   100份
プラニツトシンナ-#106)          100份其中5)是大日本涂料(株)制的丙烯酸类涂料， 6)是该社制的稀料。
在100℃干燥40分钟以后，用JISK5400方法进行方格(基盘目)实验，用实验后的涂膜的残留数评价。100/100表示粘合性良好，0/100表示膜被完全剥落。结果如表7所示。〔成形性实验〕(成形品的表面成形性)
对连续脱膜性实验的第一次脱膜后的聚氨酯成形体通过目视观察表面成形性，按如下所示标准进行评价。结果如表7所示。
A：表面成形状态良好
B：在表面能见到部分小孔(pin hole)
C：表面上全部是小孔实施例2-21
如表1-5所示变换含有硅的化合物、含有硅和/或氟的化合物、硬化促进剂、溶剂的组成，和实施例1同样调制成本发明的脱膜剂。如表1-5所示变换硬化条件，和实施例1同样形成硬化膜。各膜的膜厚如表1-5所示。
                             表1
                       表2
Figure A9419424400341
                          表3
                                   表4
Figure A9419424400361
                              表5
Figure A9419424400371
进行和实施例1同样的连续脱膜性实验、涂覆性实验和成形性实验。
另外，在实施例8中，使用己烷和二氯一氟乙烷(HCFC-141b)50∶50(重量比)的混合物作为溶剂。实施例9中，溶剂使用二甲苯和以所示的环状聚二甲基硅氧烷50∶50(重量比)的混合物。另外，在实施例11中使用的含有硅和/或氟的化合物FOMBLINZ DOL是日本モンテジソン制的化合物(在全氟代聚醚的两末端有烷氧基的化合物)。实施例14和16中使用的含有硅和/或氟的化合物是如表4所示的3种化合物的组合。
这些结果如表7所示。比较例1-8
用表6所示的成份和实施例1同样调制脱膜剂。如表6所示变换硬化条件，和实施例1同样形成硬化膜。各硬化膜的膜厚如表6所示。
                        表6
Figure A9419424400391
对这些进行与实施例1同样的连续脱膜性实验、涂覆性实验和成形性实验。
比较例5中使用的SH-200350CS是东レダウコ-ニングシリコ-ン(株)制的二甲基硅氧烷油，比较例6中使用的SH-7020是东レダウコ-ニングシリコ-ン(株)制的硅蜡。
这些结果如表7所示。另外在连续脱膜性实验的评价中，D为当时的脱膜次数，在括号内表示。
                                     表7
                连续脱膜性   涂覆性   成形性
第1次 第10次 第30次 第50次
实施例1     A     A     A     A   100/100     A
   ″  2     A     A     A     B   100/100     A
   ″  3     A     A     A     A   100/100     A
   ″  4     A     A     A     B   100/100     A
   ″  5     A     A     A     A   100/100     A
   ″  6     A     A     A     A   100/100     A
   ″  7     A     A     A     A   100/100     A
   ″  8     A     A     A     A   100/100     A
   ″  9     A     A     A     A   100/100     A
   ″ 10     A     A     A     A   100/100     A
   ″ 11     A     A     A     A   100/100     A
   ″ 12     A     A     A     B   100/100     A
   ″ 13     A     A     A     B   100/100     A
   ″ 14     A     A     A     B   100/100     A
   ″ 15     A     A     A     A   100/100     A
   ″ 16     A     A     A     B   100/100     A
   ″ 17     A     A     B     B   100/100     A
   ″ 18     A     A     A     B   100/100     A
   ″ 19     A     A     B     B   100/100     A
   ″ 20     A     A     B     B   100/100     A
   ″ 21     A     A     A     A   100/100     A
 比较例1     A     A     B   D(35)   90/100     A
   ″  2     A     B   D(21)     -   50/100     B
   ″  3     A   D(8)     -     -   0/100     C
   ″  4     A   D(7)     -     -   0/100     C
   ″  5     C   D(2)     -     -   0/100     C
   ″  6     B   D(5)     -     -   0/100     B
   ″  7     B   D(2)     -     -   0/100     B
   ″  8     A     A     B   D(30)   80/100     A
从表7所示的结果可知，如利用本发明的脱膜剂则也包含不使用硬化促进剂的情况，在连续脱膜性实验、涂覆性实验、成形性实验中的任一项中都能得到良好的结果。
本发明的脱膜剂脱膜性能优良，脱膜寿命长，而且成形品的表面成形性良好，因为在成形品表面几乎没有粘附，所以不会使成形品的涂覆性等二次加工性降低。

Claims (7)

1.一种脱膜剂，由(A)以通式(I)
           R1nSiR2 4-n    (I)〔式中，  R1表示
Figure A9419424400021
(其中，R3、R4分别是碳原子数1-4的烃基)， R2表示碳原
子数1-4的烃基或者卤代烃基，n是3或者4〕
表示的含有硅的化合物及，
(B)1分子内含有2个以上羟基或者烷氧基的含有硅和/或氟的化合物组成。
2.权利要求1中记载的脱膜剂，其中含有硅的化合物(A)及含有硅和/或氟的化合物(B)的重量比是1/99-80/20。
3.权利要求1或2中记载的脱膜剂，其中含有硅的化合物(A)是由通式(II)：
      R1nSiR2 4-n    (II)
〔式中，  R1表示
Figure A9419424400022
(其中，R3、R4分别表示碳原子数1-4的烃基)，R2表示碳原子数1-4的烃基或者卤代烃基，n是3或4〕表示的化合物。
4.权利要求1-3中任一项记载的脱膜剂，其中含有硅和/或氟的化合物(B)是从以下化合物组中选出的至少一种，以用通式(III)：
           RfA4A5            (III)(式中，Rf表示碳原子数6-21的全氟代烷基，A4表示碳原子数1-6的亚烷基，A5表示表示的化合物20重量％及以通式(IV)：
         A6OA7A8    (IV)(式中， A6表示氢原子或者碳原子数1-4的烃基，A7表示碳原子数1-6的亚烷基，A8表示
Figure A9419424400032
表示的化合物2重量％作为共聚成分的数均分子量为1000以上的共聚物、以通式(V)：
Figure A9419424400041
〔式中，j是正整数，K表示0或者正整数，j+K的平均值为10以上，优选20-5000，X1、X2表示-OH、-OR12、-R13NH2、-R14OH、-R15COOH、-R15SH或者-R12，X3表示-OH、-OR12、-R13NH2、-R14OH、-R15COOH或者-R15SH(但当K为0时X1、X2均为-OH或-OR12，当K不为0时，X1、X2、X3中至少2个是-OH或-OR12，R12是碳原子数1-4的烷基，卤代烷基或苯基， R13是碳原子数1-10的亚烷基或R16NHCH2CH2-(R16是碳原子数1-4的亚烷基)，R14表示
Figure A9419424400042
(其中，a是0或1-15的整数，b是0或1-15的整数， c是1-10的整数，d是1-5的整数)，R15是碳原子数1-10的亚烷基)，R5、R6、R7、R8、R9、 R10、R11表示碳原子数1-4的烷基、卤代烷基或苯基〕表示的化合物、以通式(VI)：
           Y1OCH2R16O-R18-R17CH2OY2    (VI)〔式中，Y1、Y2分别表示氢原子或者碳原子数1-4的烃基，R16表示-CF2-、-CF2CF2-或者 ，R17表示-CF2、-CF2CF2-或
Figure A9419424400052
，R18是从由-(CF2O)s′-、-
Figure A9419424400054
-组成的组中选出的结构单元的至少1种(R19是
Figure A9419424400055
-或者-CF2CF2CF2-，S1+S2+S3平均为5以上，优选10-200)〕表示的化合物及、
以通式(VII)：
Figure A9419424400057
(式中，Rf表示碳原子数6-21的全氟代烷基，A1表示碳原子数2-6的亚烷基，A2表示氢原子或碳原子数1-4的烷基，A3表示碳原子数1-4的烷基，S6是2或3)表示的化合物。
5.权利要求1-4中任一项记载的脱膜剂，其中含有硅和/或氟的化合物(B)是由通式(VIII)：(式中，R5、R6分别表示碳原子数1-4的烷基或卤代烷基或苯基，X4、X5均为氢原子或碳原子数1-4的烷基，m为平均值10以上，优选20-5000)表示的化合物。
6.一种硬化膜，是通过将权利要求1-5中任一项记载的含有硅的化合物及含有硅和/或氟的化合物涂覆在模具内面，使之硬化得到的硬化膜。
7.一种成形方法，是通过将权利要求1-6中任一项记载的含有硅的化合物和含有硅和/或氟的化合物涂覆在模具内面，使之硬化，在模具内形成硬化膜以后，将成形用组合物充填在该模具内成形为成形品，将成形品从该模具内脱膜的成形方法。
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