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    • 2. 发明申请
    • PROCESS FOR THE PURIFICATION OF POLYOL PFPE DERIVATIVES
    • 多元醇PFPE衍生物的纯化方法
    • WO2010130628A1
    • 2010-11-18
    • PCT/EP2010/056185
    • 2010-05-06
    • SOLVAY SOLEXIS S.p.A.TONELLI, Claudio Adolfo PietroVEZZULLI, Graziano GiuseppePICOZZI, RosaldoGAVEZOTTI, Piero
    • TONELLI, Claudio Adolfo PietroVEZZULLI, Graziano GiuseppePICOZZI, RosaldoGAVEZOTTI, Piero
    • C08G65/30
    • C08G65/007C08G65/30
    • The invention pertains to a process for the purification of a polyol (per)fluoropolyether derivative [polyol (P)], said polyol (P) comprising one or more hydroxyl (per)fluoropolyether derivatives [PFPEs (OH)] comprising at least one (per)fluoropolyoxyalkylene chain (chain R f ) and at least one end-group having formula -CF 2 CH 2 OCH 2 CH(OH)CH 2 OCH 2 CH(OH)CH 2 OH (t 3 ), from a mixture of hydroxyl (per)fluoropolyether derivatives [mixture (M)], said mixture (M) comprising said polyol (P) and at least one hydroxyl (per)fluoropolyether derivative [PFPE (OH)] different from polyol (P) and comprising at least one (per)fluoropolyoxyalkylene chain (chain R f ) and at least one end-group selected from those having formulae -CF 2 CH 2 OH (t 1 ) and -CF 2 CH 2 OCH 2 CH(OH)CH 2 OH (t 2 ), said process comprising the following steps: step 1 : reacting the mixture (M) with a ketone and/or an aldehyde so as to yield corresponding mixture of cyclic ketal/acetal (per)fluoropolyether derivatives [PFPEs (OH) p ] [protected mixture (P)]; step 2: submitting the protected mixture (P) to adsorption on silica gel so as to yield an adsorbed protected product [adsorbed product (P p )] and then recovering a desorbed protected product [desorbed product (P p )] by subsequent desorption from silica gel of said adsorbed product (P p ); step 3: distilling the desorbed product (P p ) under reduced pressure so as to isolate a protected product residue [product (P r )]; step 4: hydrolyzing the product (P r ) so as to obtain polyol (P).
    • 本发明涉及纯化多元醇(全)氟聚醚衍生物[多元醇(P)]的方法,所述多元醇(P)包含一种或多种羟基(全)含氟聚醚衍生物[PFPE(OH)],其包含至少一种( (OH)CH 2 OH(t3)的至少一个末端基团,由羟基(全)氟代聚醚衍生物[混合物(M)]的混合物,所述混合物 (P)和至少一种不同于多元醇(P)的羟基(全)氟聚醚衍生物[PFPE(OH)]并且包含至少一个(全)氟聚氧化烯链(链Rf)和至少一个末端 - 基团选自具有式-CF 2 CH 2 OH(t 1)和-CF 2 CH 2 OCH 2 CH(OH)CH 2 OH(t 2)的那些,所述方法包括以下步骤:步骤1:使混合物(M)与酮和/或醛反应, 产生相应的环缩酮/缩醛(全)氟代聚醚衍生物[PFPE(OH)p] [保护的混合物(P) ]。 步骤2:将保护的混合物(P)提交到硅胶上吸附,得到吸附的保护产物[吸附产物(Pp)],然后通过随后的硅胶解吸回收解吸的保护产物[解吸产物(Pp)] 的所述吸附产物(Pp); 步骤3:在减压下蒸馏除油产物(Pp),以分离受保护的产物残渣[产物(Pr)]; 步骤4:水解产物(Pr)以获得多元醇(P)。
    • 3. 发明申请
    • PROCESS FOR THE MANUFACTURE OF POLYOL PERFLUOROPOLYETHER DERIVATIVE
    • 聚氟乙烯衍生物的制备方法
    • WO2009043928A1
    • 2009-04-09
    • PCT/EP2008/063278
    • 2008-10-03
    • SOLVAY SOLEXIS S.P.A.TONELLI, ClaudioVEZZULLI, Graziano, GiuseppePICOZZI, RosaldoGAVEZOTTI, PieroDI MEO, Antonella
    • TONELLI, ClaudioVEZZULLI, Graziano, GiuseppePICOZZI, RosaldoGAVEZOTTI, PieroDI MEO, Antonella
    • C08G65/00C08G65/48
    • C07C41/26C07C43/126C08G65/007C08G65/22C08G65/2639C08G65/3312C10M2211/063
    • The invention pertains to a process for the manufacture of a polyol (per)fluoropolyether derivative [polyol PFPE (PFPE-OH)], said process comprising: 1. reacting at least one triol having two protected hydroxyl functions and a free hydroxyl group [protected triol (PT)] with an activating agent, to yield an activated protected triol [activated protected triol (APT)]; 2. reacting said activated protected triol with a functional (per)fluoropolyether derivative of formula (Ia) [functional PFPE (E)], wherein: R f represents a fluoropolyoxyalkene chain (chain R f ), i.e. a fluorocarbon segment comprising ether linkages in main chain; T 1 and T 2 , equal to or different from each other, are independently selected from - non-functional groups of formula: -CF 3 , -CF 2 -CF 3 , -CF 2 CI, -CF 2 CF 2 CI, -CF 2 -COF, -COF : and - functional hydroxyl groups comprising at least one hydroxyl group, with the provisio that at least one of T 1 and T 2 is a functional hydroxyl group as above detailed; to yield a protected polyol (per)fluoropolyether derivative [protected polyol PFPE (p-PFPE-OH)]; 3. deprotecting said protected polyol PFPE (p-PFPE-OH) to yield the polyol PFPE (PFPE-OH).
    • 本发明涉及制备多元醇(全)氟聚醚衍生物[多元醇PFPE(PFPE-OH)]的方法,所述方法包括:使至少一种具有两个保护的羟基官能团和游离羟基的三醇[保护的 三醇(PT)]与活化剂反应,得到活化的保护三醇[活性保护三醇(APT)]; 2.使所述活化的被保护的三醇与式(Ia)的功能性(全)氟聚醚衍生物[功能性PFPE(E)]反应,其中:Rf表示氟聚氧亚烷基链(链Rf),即在主链中包含醚键的氟烃链段 ; T1和T2彼此相同或不同,独立地选自以下的非官能团:-CF 3,-CF 2 -CF 3,-CF 2 Cl,-CF 2 CF 2 Cl,-CF 2 -COF,-COF:和 - 官能羟基 包含至少一个羟基的基团,条件是T1和T2中的至少一个是如上详述的官能羟基; 得到受保护的多元醇(全)氟聚醚衍生物[保护的多元醇PFPE(p-PFPE-OH)]; 3.将保护的多元醇PFPE(p-PFPE-OH)脱保护,得到多元醇PFPE(PFPE-OH)。
    • 5. 发明申请
    • FLUORINATED POLYURETHANE COMPOSITION
    • 氟化聚氨酯组合物
    • WO2008138927A1
    • 2008-11-20
    • PCT/EP2008/055838
    • 2008-05-13
    • SOLVAY SOLEXIS S.p.A.RUSSO, AntonioGAVEZOTTI, PieroQUALLO, Michael
    • RUSSO, AntonioGAVEZOTTI, PieroQUALLO, Michael
    • C08G18/08C08G18/12C08G18/32C08G18/50C08L75/04
    • C08G18/0814C08G18/0823C08G18/3206C08G18/3819C08G18/3893C08G18/5015C08G18/755C08G18/80C08L33/16D06M15/277D06M15/576D06M2200/01D06M2200/10D06M2200/11D06M2200/12C08L75/04C08L2666/06
    • The invention pertains to a composition useful for imparting durable stain repellence and soil release properties to textile substrates, said composition comprising: (A) at least one fluorinated ionisable polyurethane polymer [polymer (PUR)] comprising at least one fluorinated block comprising a fluoropolyoxyalkene chain [chain (R of )], and at least one functional block comprising an hydrocarbon chain [chain (R HC )] having from 2 to 14 carbon atoms, optionally comprising one or more aromatic or cycloaliphatic group, said chain (R HC ) comprising at least one ionisable group, said blocks being linked by urethane moieties of formula (I): wherein E is a divalent hydrocarbon carbon group, linear or branched, optionally comprising aromatic rings, said polymer (PUR) being free from perfluoroalkyl chains [chain (R f )]; (B) at least one fluorocarbon polymer [polymer (F)] comprising at least one perfluoroalkyl chain [chain (R f )] linked by one or more ester moiety of formula (II) and/or urethane moiety of formula (III) and/or urea moiety of formula (IV): (C) at least one crosslinking agent. Still object of the invention are the use of said composition for treating textile substrates and the textile substrates obtained therefrom.
    • 本发明涉及可用于赋予织物基质持久的防污性和去污性的组合物,所述组合物包含:(A)至少一种含氟可电离聚氨酯聚合物[聚合物(PUR)],其包含至少一个含氟聚氧亚烷基链的氟化嵌段 [链(R))和至少一个包含具有2至14个碳原子的烃链[链(R)C H])的官能团,任选地包含一个 或更多的芳香族或脂环族基团,所述链(R CH)包含至少一个可离子化基团,所述嵌段通过式(I)的氨基甲酸酯部分连接:其中E是二价烃碳基,线性 或支链的,任选地包含芳香环,所述聚合物(PUR)不含全氟烷基链[链(R))。 (B)包含至少一个由一个或多个式(II)的酯部分和/或氨基甲酸酯连接的全氟烷基链[链(R))的氟碳聚合物[聚合物(F)]] 式(III)的部分和/或式(IV)的脲部分):(C)至少一种交联剂。 本发明的另一目的是使用所述组合物来处理织物基材和由其获得的织物基材。
    • 8. 发明申请
    • PROCESS FOR THE PURIFICATION OF POLYOL PFPE DERIVATIVES
    • 多元醇PFPE衍生物的纯化方法
    • WO2010130625A1
    • 2010-11-18
    • PCT/EP2010/056177
    • 2010-05-06
    • SOLVAY SOLEXIS S.P.A.VEZZULLI, Graziano GiuseppeGAVEZOTTI, PieroMUTTA, FabrizioTONELLI, Claudio Adolfo Pietro
    • VEZZULLI, Graziano GiuseppeGAVEZOTTI, PieroMUTTA, FabrizioTONELLI, Claudio Adolfo Pietro
    • C08G65/30
    • C08G65/007C08G65/30
    • The invention pertains to a process for the purification of a polyol (per)fluoropolyether derivative [polyol (P)], said polyol (P) comprising one or more hydroxyl (per)fluoropolyether derivatives [PFPE (OH)] comprising at least one (per)fluoropolyoxyalkylene chain (chain R f ) and at least one end-group having formula -CF 2 CH 2 OCH 2 CH(OH)CH 2 OCH 2 CH(OH)CH 2 OH (t3), from a mixture of hydroxyl (per)fluoropolyether derivatives [mixture (M)], said mixture (M) comprising said polyol (P) and at least one hydroxyl (per)fluoropolyether derivative [PFPE (OH)] different from polyol (P) and comprising at least one (per)fluoropolyoxyalkylene chain (chain Rf) and at least one end-group selected from those having formulae -CF 2 CH 2 OH (t 1 ) and -CF 2 CH 2 OCH 2 CH(OH)CH 2 OH (t 2 ), said process comprising the following steps: step 1 : reacting the mixture (M) with a ketone and/or an aldehyde so as to yield corresponding mixture of cyclic ketal/acetal (per)fluoropolyether derivatives [PFPEs (OH) p ] [protected mixture (P)]; step 2: molecular distillation of the protected mixture (P) so as to isolate a protected product heavy residue [product (P r )]; step 3: hydrolyzing the product (P r ) so as to yield a deprotected product [product (P d )]; step 4: distillation under reduced pressure of the product (P d ) so as to obtain polyol (P).
    • 本发明涉及纯化多元醇(全)氟聚醚衍生物[多元醇(P)]的方法,所述多元醇(P)包含一种或多种羟基(全)含氟聚醚衍生物[PFPE(OH)],其包含至少一种( (OH)CH 2 OH(t3)的至少一个末端基团,由羟基(全)氟代聚醚衍生物[混合物(M)]的混合物,所述混合物 (P)和至少一种不同于多元醇(P)的羟基(全)氟聚醚衍生物[PFPE(OH)]并且包含至少一个(全)氟聚氧化烯链(链Rf)和至少一个末端 - 基团选自具有式-CF 2 CH 2 OH(t 1)和-CF 2 CH 2 OCH 2 CH(OH)CH 2 OH(t 2)的那些,所述方法包括以下步骤:步骤1:使混合物(M)与酮和/或醛反应, 产生相应的环缩酮/缩醛(全)氟聚醚衍生物[PFPE(OH)p] [保护的混合物(P) ]。 步骤2:保护的混合物(P)的分子蒸馏,以分离受保护的产物重残渣[产物(Pr)]; 步骤3:水解产物(Pr)以产生脱保护的产物[产物(Pd)]; 步骤4:在减压下蒸馏产物(Pd),得到多元醇(P)。
    • 9. 发明申请
    • PROCESS FOR THE PURIFICATION OF POLYOL PFPE DERIVATIVE
    • 多元醇PFPE衍生物的纯化方法
    • WO2009112578A1
    • 2009-09-17
    • PCT/EP2009/052999
    • 2009-03-13
    • SOLVAY SOLEXIS S.p.A.TONELLI, ClaudioVEZZULLI, Graziano, GiuseppePICOZZI, RosaldoGAVEZOTTI, Piero
    • TONELLI, ClaudioVEZZULLI, Graziano, GiuseppePICOZZI, RosaldoGAVEZOTTI, Piero
    • C08G65/30
    • C08G65/30C08G65/007C08G65/22C08G65/24
    • The invention pertains to a process for the purification of a tetraol PFPE derivative [tetraol (T)] of formula (I): HO-CH 2 -CH(OH)-CH 2 -O-CH 2 -CF 2 -O-R f -CF 2 -CH 2 O-CH 2 -CH(OH)-CH 2 OH (I), wherein R f represents a fluoropolyoxyalkene chain (chain R f ), i.e. a fluorocarbon segment comprising ether linkages in main chain, from a mixture of hydroxyl (per)fluoropolyether derivatives [mixture (M)], said mixture comprising said tetraol (T) and at least one hydroxyl (per)fluoropolyether [PFPE (OH)] comprising a chain R f terminated with at least one end group of formula: -CF 2 CH 2 OH) -CF 2 CH 2 O-CH(OH)-CH 2 -O-CH 2 -CH(OH)-CH 2 OH; said process comprising: step 1 : reacting the mixture (M) with ketones and/or aldehydes so as to selectively protect couples of hydroxyl groups on vicinal carbon atoms by forming corresponding cyclic ketal/acetal derivatives, so as to yield a protected mixture [mixture (P)]; step 2: reacting residual hydroxyl groups of the mixture (P) with suitable functionalizing agents enabling substantial volatility modification, so as to obtain a functionalized protected mixture [mixture (P f )]; step 3: fractional distillation of the mixture (P f ) so as to isolate the cyclic acetal/ketal derivatives of tetraol (T); step 4. hydrolyzing the acetal/ketal derivatives of tetraol (T) so as to recover pure tetraol (T).
    • 本发明涉及纯化式(I)的四醇PFPE衍生物[四醇(T))的方法:HO-CH2-CH(OH)-CH2-O-CH2-CF2-O-Rf-CF2-CH2O -CH 2 -CH(OH)-CH 2 OH(I),其中R f表示氟代聚氧亚烷基链(链Rf),即包含主链中的醚键的氟烃链段,由羟基(全)氟聚醚衍生物的混合物[混合物(M) ],所述混合物包含所述四醇(T)和至少一种羟基(全)氟聚醚[PFPE(OH)),其包含用至少一个具有下列结构的末端基团终止的链Rf:-CF 2 CH 2 OH)-CF 2 CH 2 O-CH(OH) CH2-O-CH2-CH(OH)-CH 2 OH; 所述方法包括:步骤1:使混合物(M)与酮和/或醛反应,以便通过形成相应的环缩酮/缩醛衍生物来选择性保护连位碳原子上的羟基,从而产生受保护的混合物[混合物 (P)]; 步骤2:使混合物(P)的残余羟基与合适的官能化试剂反应,使得能够进行实质的挥发性改性,以获得官能化的保护的混合物[混合物(Pf)]; 步骤3:分馏混合物(Pf),以分离四醇(T)的环状缩醛/缩酮衍生物; 步骤4.水解四醇(T)的缩醛/缩酮衍生物,以回收纯四醇(T)。