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New block copolymers for prodn. of films, sealants and coatings - contg. as one block, polymer of cyclic aliphatic carbonate or copolymer with cyclic aliphatic ester and as other block, poly:siloxane

机译：新型嵌段共聚物薄膜，密封剂和涂料的制造-续作为一种嵌段，是环状脂族碳酸酯的聚合物或与环状脂族酯的共聚物;作为另一种嵌段，是聚：硅氧烷

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Block copolymers of formula A-B-A (I) are new where A = polymer of cyclic, aliphatic carbonate(s) or carbonate(s) and ester(s) (II); B = polysiloxane block. Prodn. of (I) is by reacting alpha,omega-dihydroxy-polysiloxane (III) with alkali metal or organo-alkali metal cpd. (IV) in aprotic organic solvent (V), then adding soln. of (II) in (V), polymerising and deactivating the active centres. Pref. block (A) is a polymer of carbonates of formula (IIA) and/or (IIB), or a copolymer with esters of formula (IIC), and block (B) is a polysiloxane of formula -O-(SiR7-O)o-; R1 = -CH2CH2CHMe-, -CH2CH2OCH2CH2OCH2CH2- (gp.b), -CH2CHMeCH2CH2CMe2CH2-, -CH2CH2O-Phe-CMe2-Phe-OCH2CH2-, -CHMeCH2O-Phe-CMe2-Phe-OCH2CHMe-, -CH2-CMe2-CH2-, gp.(i) or -CH2-C(Et)(n-Bu)-CH2- (with Phe = p-phenylene); R2 = linear 4-12C alkylene, a gp. of formula (b) or -CH2CH2OCH2CH2-; R3-R6 = H, 1-6C alkyl or alkoxy, 3-6C alkenyl or (2-6C alkenoxy)-(1-6C alkyl); m, n = 0, 1, 2, 3, 4, 5 or 6. R7 = 1-20C linear alkyl, 3-12C branched alkyl or 6-20C aryl; o = 3-1400. Pref., (A) is polyneopentyl glycol carbonate or a copolymer of neopentyl glycol carbonate and epsilon-caprolactone, and (B) is polydimethylsiloxane. Pref., block (A) and (B) have Mn 2000-50,000 and 500-50,000 respectively. Polymerisation is effected in toluene at -20 to +50 deg. C, and polymerisation centres are then deactivated, e.g. with MeOH/HCl. USE/ADVANTAGE - (I) are useful for the prodn. of films, sealants and coatings, esp. for applications requiring improved long-term properties, and for the prodn. of resin-like, thermoplastic packaging materials. In an example, a soln. of 0.11 g OH-terminated polydimethylsiloxane (Mn = 900) in 20 ml toluene was mixed with 2.5 mol 0.1M sec.-BuLi soln. and stirred for 30 mins., then a soln. of 5 g neopentyl glycol carbonate in 40 ml toluene was added and the mixt. was allowed to react for 16 hrs. Mixt. was worked up by deactivation with 2 ml 5% H3PO4/MeOH soln. and pptn. in 150 ml MeOH to give (I) in 89 yield. Prod. had Mn = 61,000.

机译：式A-B-A（I）的嵌段共聚物是新的，其中A ＝环状，脂族碳酸酯或碳酸酯和酯的聚合物（II）; B ＝聚硅氧烷嵌段。产品（I）的α是使α，ω-二羟基聚硅氧烷（III）与碱金属或有机碱金属cpd反应。（IV）在非质子有机溶剂（V）中，然后加入soln。（V）中的（II）中的化合物，使活性中心聚合并失活。首选嵌段（A）是式（IIA）和/或（IIB）的碳酸酯的聚合物，或与式（IIC）的酯的共聚物，并且嵌段（B）是式-O-（SiR 7 -O）的聚硅氧烷o-; R1 = -CH2CH2CHMe-，-CH2CH2OCH2CH2OCH2CH2-（gp.b），-CH2CHMeCH2CH2CMe2CH2-，-CH2CH2O-Phe-CMe2-Phe-OCH2CH2-，-CHMeCH2O-Phe-CMe2-Phe-OCH2CHMe2-，-CH2CH2CH2CHMe- ，gp。（i）或-CH 2 -C（Et）（n-Bu）-CH 2-（其中Phe ＝对亚苯基）; R 2 ＝线性4-12C亚烷基，gp。式（b）或-CH 2 CH 2 OCH 2 CH 2-; R3-R6 ＝ H，1-6C烷基或烷氧基，3-6C烯基或（2-6C烯氧基）-（1-6C烷基）; m，n ＝ 0、1、2、3、4、5或6。R 7 ＝ 1-20C直链烷基，3-12C支链烷基或6-20C芳基; o = 3-1400。优选，（A）为聚新戊二醇碳酸酯或碳酸新戊二醇与ε-己内酯的共聚物，（B）为聚二甲基硅氧烷。优选地，嵌段（A）和（B）的Mn分别为2000-50,000和500-50,000。聚合在-20至+ 50℃下在甲苯中进行。 C，然后使聚合中心失活，例如用MeOH / HCl。使用/优势-（I）对产品有用。薄膜，密封剂和涂料的生产，尤其是适用于需要改善长期性能的应用，以及产品类树脂的热塑性包装材料。在一个例子中，是Soln。将在20ml甲苯中的0.11g OH-封端的聚二甲基硅氧烷（Mn ＝ 900）与2.5mol 0.1M sec-BuLi溶液混合。搅拌30分钟，然后搅拌。加入5克新戊二醇碳酸酯在40毫升甲苯中的溶液，并混合。让其反应16小时。混蛋通过用2 ml 5％H3PO4 / MeOH溶液失活来后处理。和pptn。在150ml MeOH中溶解，得到（I），产率为89。产品Mn ＝ 61,000。

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公开/公告号DE4131187A1

专利类型
公开/公告日1993-03-25

原文格式PDF
申请/专利权人 BAYER AG 5090 LEVERKUSEN DE;
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申请/专利号DE19914131187
发明设计人 SYLVESTER GERD DIPL.-CHEM. DR. 5090 LEVERKUSEN DE;HOECKER HARTWIG PROF. DIPL.-CHEM. DR. 5100 AACHEN DE;KEUL HELMUT DIPL.-CHEM. DR.;LEITZ EDGAR DIPL.-CHEM. DR. 4047 DORMAGEN DE;MUELLER ACHIM DIPL.-CHEM. 5102 WUERSELEN DE;
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申请日1991-09-19
分类号C08G77/448;
国家 DE
入库时间 2022-08-22 05:01:39

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