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    • 1. 发明申请
    • COMPOSITE FILLER PARTICLES AND PROCESS FOR THE PREPARATION THEREOF
    • 复合填料颗粒及其制备方法
    • WO2013087223A1
    • 2013-06-20
    • PCT/EP2012/005206
    • 2012-12-17
    • DENTSPLY DETREY GMBH
    • STELZIG, SimonKEMPTER, JörgNOERPEL, StephanieKLEE, Joachim, E.FACHER, AndreasWALZ, UweWEBER, Christoph
    • A61K6/083A61K6/02
    • C09D143/04A61K6/0008A61K6/0076A61K6/0085A61K6/0091A61K6/0215A61K6/024A61K6/025A61K6/083B01J2/16B05D7/24C01P2004/61C03C14/008C03C17/00C03C17/30C03C2214/12C08K3/40C08K5/5419C09C1/40C09C3/00C09C3/006C09C3/045C09C3/08C09C3/12C08L33/00
    • A process for the preparation of composite filler particles, comprising: (a) coating a particulate filler having a median particle size (D50) of from 1 to 1200 nm with a coating composition containing a film-forming agent forming a coating layer on the surface of the particulate filler, said coating layer displaying reactive groups on the surface of the coating layer, said reactive groups being selected from addition polymerizable groups and step-growth polymerizable groups, thereby forming a coated particulate filler; subsequently or concurrently (b) agglomerating the coated particulate filler, optionally in the presence of a further crosslinking agent and optionally in the presence of a further particulate filler not displaying reactive groups, for providing a granulation of the coated particulate filler wherein the granulation contains the coated particulate filler particles and the optional further particulate filler particles separated from and connected to each other by at least one coating layer, whereby the at least one coating layer may be crosslinked by crosslinking groups obtained by reacting the reactive groups and optionally a further crosslinking agent; (c) optionally milling, classifying and/or sieving the granulation of the coated particulate filler; and (d) optionally further crosslinking the granulation of the coated particulate filler; for providing composite filler particles having a median particle size (D50) of from 1 to 70 μιτι, wherein reactive groups are transformed into crosslinking groups obtained by reacting reactive groups and optionally a further crosslinking agent, and wherein the particulate filler is the main component by volume of the composite filler particles.
    • 一种制备复合填料颗粒的方法,包括:(a)用包含在表面上形成涂层的成膜剂的涂料组合物涂覆中等颗粒尺寸(D50)为1至1200nm的颗粒填料 所述涂层在涂层的表面上显示反应性基团,所述反应性基团选自加成聚合基团和步进生长可聚合基团,从而形成涂布的颗粒填料; 随后或同时(b)任选地在另外的交联剂的存在下和任选地在不显示反应性基团的另外的颗粒填料的存在下任选地使涂覆的颗粒填料附聚,以提供涂覆的颗粒填料的造粒,其中造粒物包含 涂覆的颗粒填料颗粒和任选的另外的颗粒填料颗粒通过至少一个涂层彼此分离和连接,由此至少一个涂层可以通过使反应基团和任选的另外的交联剂反应获得的交联基团交联 ; (c)任选地研磨,分级和/或筛分涂覆的颗粒填料的造粒物; 和(d)任选地进一步交联涂覆的颗粒填料的造粒物; 用于提供中值粒径(D50)为1至70μmolataotaotaota的复合填料颗粒,其中反应性基团转化为通过反应性基团和任选另外的交联剂反应获得的交联基团,并且其中颗粒填料是主要组分 复合填料颗粒的体积。
    • 2. 发明申请
    • DENTAL COMPOSITION
    • 牙科成分
    • WO2012119793A2
    • 2012-09-13
    • PCT/EP2012/001103
    • 2012-03-12
    • DENTSPLY DETREY GMBHSTELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • STELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • A61K6/083
    • A61K6/083
    • Dental composition selected from a dental cement and a dental adhesive, comprising (i) a water-soluble polymerizable compound of the following formula (1), AX n (1) wherein A is a straight chain or branched linker group containing at least n nitrogen atoms, and optionally one or more acidic groups; X are moieties containing a polymerizable double bond, which X may be the same or different and are represented by the following formula (2), whereby a moiety X of formula (2) is linked to the nitrogen atom of an amino group or a carboxamide group of A, formula (2) wherein R 1 and R 2 are independent from each other and represent a hydrogen atom, a C 1-6 alkyl group or a group -(CH2) m -COOM, wherein M is a hydrogen atom or a metal atom, and m is an integer of from 0 to 6, L is a bond or a C 1-6 alkylene group; and is an integer of at least 1; which is obtainable by a process comprising (a) a step of a step-growth polymerization of a mixture containing a polyamine and a compound having at least two carboxylic acid groups or an anhydride thereof, optionally in the presence of a compound of the following formula (5) for obtaining a polyamide: formula (5) wherein R 1 and R 2 are as defined above, and Y 1 is a leaving group or Y 1 forms an hydrolysable intramolecular group together with a carboxyl group present in R 1 or R 2 and the adjacent carbonyl group; and (b) a step of introducing moieties of the formula (2) by reacting the polyamide obtained in step (i) with a compound of formula (5) wherein Y1 is a leaving group and R 1 and R 2 are as defined above; or (c) a step of reacting a mixture containing a polyamine and a compound of formula (5) for obtaining an amine reaction product; and (d) a step of a step-growth polymerization of a mixture containing the amine reaction product obtained in (c) and a compound having at least two carboxylic acid groups or an anhydride thereof for obtaining the water-soluble polymerizable compound of the formula (1), an initiator system; optionally a polyacidic polymer; and optionally water and/or a water soluble solvent, optionally a particulate filler.
    • 选自牙科粘固剂和牙科粘合剂的牙科成分,其包含(i)下式(1)的水溶性可聚合化合物,AXn(1)其中A是至少含有n个氮原子的直链或支链连接基团 ,和任选的一个或多个酸性基团; X是含有可聚合双键的部分,X可以相同或不同,由下式(2)表示,其中式(2)的X部分与氨基或羧酰胺的氮原子连接 A组,式(2)其中R 1和R 2彼此独立并且表示氢原子,C 1-6烷基或基团 - (CH 2)m -COOM,其中M是氢原子或金属原子 m为0〜6的整数,L为碳原子数为1〜6的亚烷基。 并且是至少为1的整数; 其可通过以下方法获得,该方法包括(a)含有多胺和具有至少两个羧酸基团的化合物或其酸酐的混合物的步进生长聚合步骤,任选地在下式的化合物 (5)其中R 1和R 2如上所定义,Y 1为离去基团或Y 1与R1或R2和相邻羰基中存在的羧基一起形成可水解的分子内基团; 和(b)通过使步骤(i)中获得的聚酰胺与式(5)的化合物反应来引入式(2)的部分的步骤,其中Y1是离去基团,R1和R2如上定义; 或(c)使含有多胺和式(5)化合物的混合物反应以获得胺反应产物的步骤; 和(d)包含(c)中得到的胺反应产物的混合物和具有至少两个羧酸基团的化合物或其酸酐的混合物的步进生长聚合步骤,以获得式(I)的水溶性聚合性化合物 (1),发起者系统; 任选的多酸聚合物; 和任选的水和/或水溶性溶剂,任选的颗粒填料。
    • 3. 发明申请
    • DENTAL COMPOSITION
    • 牙科成分
    • WO2012052160A1
    • 2012-04-26
    • PCT/EP2011/005232
    • 2011-10-18
    • DENTSPLY DETREY GMBHSTELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • STELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • A61K6/02A61K6/083C07C233/31
    • A61K6/083A61K6/0023A61K6/0835C07C233/20C08L33/00
    • Dental composition comprising a water-soluble polymerizable compound of the following formula (1): wherein A is a linear or branched linker group represented by the following formula (3), wherein the nitrogen atom of at least two of the termini forms an amide bond with an X moiety; wherein R' represents a hydrogen atom or a substituted or unsubstituted aliphatic or cycloaliphatic hydrocarbon group, wherein each R may be the same or different L 1 , L 2 , and L 3 which may be the same or different, independently represent a single bond, or a C 2-20 straight-chain, branched or cyclic hydrocarbon group optionally containing from 1 to 6 heteroatoms selected from nitrogen and oxygen in the backbone of the hydrocarbon group, and optionally from 1 to 6 functional groups selected from carboxylic acid groups or a salt thereof, hydroxyl groups, thiol groups and amino groups, and in case a plurality of L 1 and L 2 are present, each of L 1 and L 2 may be the same or different; Q 1 and Q 2 , which may be the same or different, independently represent a single bond or a linkage selected from an amide, a urethane, a urea and a thiourea linkage; k is an integer of at least 0, X are moieties containing a polymerizable double bond and forming an amide bond with a nitrogen atom of A, wherein each X may be the same or different and are represented by the following formula (2): wherein R 1 and R 2 are independent from each other and represent a hydrogen atom, a C 1-6 alkyl group or a group -(CH 2 ) m -COOM, wherein M represents a hydrogen atom or a metal atom, m is an integer of from 0 to 6, L is a bond or a C 1-6 alkylene group; and n is an integer of at least 2; (ii) an initiator system; optionally a polyacidic polymer; optionally water and/or a water soluble solvent; and optionally a particulate filler.
    • 1.一种牙科用组合物,其含有下述式(1)所示的水溶性聚合性化合物:式中,A为下述通式(3)所示的直链或支链连接基团,其中,所述末端中的至少2个的氮原子形成酰胺键 与X部分; 其中R'表示氢原子或取代或未取代的脂族或脂环族烃基,其中每个R可以相同或不同,可相同或不同的L1,L2和L3独立地表示单键,或C2 -20个直链,支链或环状烃基,任选地含有1至6个选自氮原子和氧的杂原子在烃基的主链中,以及任选地1-6个选自羧酸基团或其盐的官能团,羟基 基团,硫醇基和氨基,并且在存在多个L1和L2的情况下,L1和L2中的每一个可以相同或不同; Q1和Q2可以相同或不同,独立地表示单键或选自酰胺,氨基甲酸酯,脲和硫脲键的键; k是至少为0的整数,X是含有可聚合双键并与A的氮原子形成酰胺键的部分,其中每个X可以相同或不同,并由下式(2)表示:其中 R 1和R 2彼此独立地表示氢原子,C 1-6烷基或基团 - (CH 2)m -COOM,其中M表示氢原子或金属原子,m表示0〜 6,L是键或C1-6亚烷基; 且n为至少2的整数; (ii)引发剂体系; 任选的多酸聚合物; 任选的水和/或水溶性溶剂; 和任选的颗粒填料。
    • 4. 发明申请
    • DENTAL CEMENT COMPOSITION
    • 牙科水泥组合物
    • WO2012052163A1
    • 2012-04-26
    • PCT/EP2011/005238
    • 2011-10-18
    • DENTSPLY DETREY GMBHSTELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • STELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • A61K6/02A61K6/083A61K6/00C07C233/09C07C233/31
    • A61K6/0835A61K6/0023A61K6/0091A61K6/09C07C233/09C07C233/20C08F122/385C08L33/00C08L75/16
    • Dental cement composition comprising (i) a particulate filler reactive with a polyacid in a cement reaction; (ii) a water-soluble polymerizable compound of the following formula (1), AXn (1) wherein A is a linker group containing at least n nitrogen atoms and optionally one or more acidic groups, X are moieties containing a polymerizable double bond and forming an amide bond with a nitrogen atom of A, which X may be the same or different and are represented by the following formula (2) wherein R 1 and R 2 are independent from each other and represent a hydrogen atom, a C 1-6 alkyl group or a group -(CH 2 ) m -Z, wherein Z is COOM, OPO 3 M 2 , PO 3 M 2 , SO 3 M, and M is independently a hydrogen atom or a metal atom, and m is an integer of from 0 to 6, L is a bond or a C 1-6 alkylene group; and n is an integer of at least 1; provided that at least one X cannot be a (meth)acryl group; and (iii) an initiator system; optionally a polyacidic polymer having polymerizable double bonds; and optionally water.
    • 牙科水泥组合物,其包含(i)在水泥反应中与多元酸反应的颗粒填料; (ⅱ)下述式(1)的水溶性聚合性化合物,其中A为含有至少n个氮原子和任意一个以上酸性基团的连接基团,X 1为含有可聚合双键的部分, 与A的氮原子形成酰胺键,X可以相同或不同,并由下式(2)表示,其中R 1和R 2彼此独立地表示氢原子,C 1-6烷基 或基团 - (CH 2)m Z,其中Z为COOM,OPO 3 M 2,PO 3 M 2,SO 3 M和M独立地为氢原子或金属原子,m为0至6的整数,L为键或C1 -6亚烷基; n为1以上的整数。 条件是至少一个X不能是(甲基)丙烯酰基; 和(iii)引发剂体系; 任选的具有可聚合双键的多酸聚合物; 和任选的水。
    • 6. 发明公开
    • DENTAL COMPOSITION
    • 牙科组合物
    • EP2629740A1
    • 2013-08-28
    • EP11771039.2
    • 2011-10-18
    • Dentsply DeTrey GmbH
    • STELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • A61K6/02A61K6/083C07C233/31
    • A61K6/083A61K6/0023A61K6/0835C07C233/20C08L33/00
    • Dental composition comprising a water-soluble polymerizable compound of the following formula (1): €ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ AX n €ƒ€ƒ€ƒ€ƒ€ƒ(1) wherein A is a straight chain or branched linker group containing least n nitrogen atoms, whereby the linker group has polyoxyalkylene and/or polyalkylene imine repeating units and optionally one or more acidic groups, X are moieties containing a polymerizable double bond and forming an amide bond with a nitrogen atom of A, wherein each X may be the same or different and are represented by the following formula (2): wherein R 1 and R 2 are independent from each other and represent a hydrogen atom, a C 1-6 alkyl group or a group -(CH 2 ) m -COOM, wherein M represents a hydrogen atom or a metal atom, m is an integer of from 0 to 6, L is a bond or a C 1-6 alkylene group; and n is an integer of at least 1; (ii) an initiator system; optionally a polyacidic polymer; optionally water and/or a water soluble solvent; and optionally a particulate filler.
    • 包含下式(1)的水溶性可聚合化合物的牙科组合物:(1)其中A 是含有至少n个氮原子的直链或支链连接基团,其中连接基团具有聚氧化烯和/或聚亚烷基亚胺重复单元和任选的一个或多个酸性基团,X是含有可聚合双键并与 A的氮原子,其中每个X可以相同或不同并且由下式(2)表示:其中R 1和R 2彼此独立并且表示氢原子,C 1-6烷基或 基团 - (CH 2)m -COOM,其中M表示氢原子或金属原子,m为0至6的整数,L为键或C 1-6亚烷基; 并且n是至少为1的整数; (ii)引发剂体系; 任选的多酸聚合物; 任选地水和/或水溶性溶剂; 和任选的颗粒填料。
    • 7. 发明公开
    • COMPOSITE FILLER PARTICLES AND PROCESS FOR THE PREPARATION THEREOF
    • 复合填料颗粒及其制备方法
    • EP2790639A1
    • 2014-10-22
    • EP12813274.3
    • 2012-12-17
    • Dentsply DeTrey GmbH
    • STELZIG, SimonKEMPTER, JörgNOERPEL, StephanieKLEE, Joachim, E.FACHER, AndreasWALZ, UweWEBER, Christoph
    • A61K6/083A61K6/02
    • C09D143/04A61K6/0008A61K6/0076A61K6/0085A61K6/0091A61K6/0215A61K6/024A61K6/025A61K6/083B01J2/16B05D7/24C01P2004/61C03C14/008C03C17/00C03C17/30C03C2214/12C08K3/40C08K5/5419C09C1/40C09C3/00C09C3/006C09C3/045C09C3/08C09C3/12C08L33/00
    • A process for the preparation of composite filler particles, comprising: (a) coating a particulate filler having a median particle size (D50) of from 1 to 1200 nm with a coating composition containing a film-forming agent forming a coating layer on the surface of the particulate filler, said coating layer displaying reactive groups on the surface of the coating layer, said reactive groups being selected from addition polymerizable groups and step-growth polymerizable groups, thereby forming a coated particulate filler; subsequently or concurrently (b) agglomerating the coated particulate filler, optionally in the presence of a further crosslinking agent and optionally in the presence of a further particulate filler not displaying reactive groups, for providing a granulation of the coated particulate filler wherein the granulation contains the coated particulate filler particles and the optional further particulate filler particles separated from and connected to each other by at least one coating layer, whereby the at least one coating layer may be crosslinked by crosslinking groups obtained by reacting the reactive groups and optionally a further crosslinking agent; (c) optionally milling, classifying and/or sieving the granulation of the coated particulate filler; and (d) optionally further crosslinking the granulation of the coated particulate filler; for providing composite filler particles having a median particle size (D50) of from 1 to 70 µm, wherein reactive groups are transformed into crosslinking groups obtained by reacting reactive groups and optionally a further crosslinking agent, and wherein the particulate filler is the main component by volume of the composite filler particles.
    • 一种用于制备复合填料颗粒的方法,包括:(a)用含有在表面上形成涂层的成膜剂的涂料组合物涂布中值粒径(D50)为1-1200nm的颗粒填料 所述涂层在所述涂层表面上显示反应性基团,所述反应性基团选自可加聚的基团和可逐步生长的可聚合基团,从而形成涂覆的颗粒状填料; 随后或同时(b)任选地在另外的交联剂存在下和任选地在另外的没有显示反应性基团的颗粒状填料的存在下附聚涂覆的颗粒状填料,以提供涂覆的颗粒状填料的造粒,其中造粒剂含有 涂覆的颗粒状填料颗粒和任选的另外的颗粒状填料颗粒通过至少一个涂层彼此分离并且彼此连接,由此所述至少一个涂层可以通过交联基团交联,所述交联基团通过反应性基团和任选的另外的交联剂 ; (c)任选研磨,分级和/或筛分涂覆的颗粒状填料的颗粒; 和(d)任选地进一步交联涂布的颗粒状填料的颗粒; 用于提供具有1至70μm的中值粒度(D50)的复合填料颗粒,其中反应性基团被转化为通过反应性基团和任选的另外的交联剂反应获得的交联基团,并且其中所述颗粒填料是 复合填料颗粒的体积。
    • 8. 发明公开
    • DENTAL COMPOSITION
    • 牙科组合物
    • EP2629741A1
    • 2013-08-28
    • EP11773194.3
    • 2011-10-18
    • Dentsply DeTrey GmbH
    • STELZIG, SimonKLEE, Joachim, E.FACHER, AndreasWEBER, Christoph
    • A61K6/02A61K6/083C07C233/31C07C233/09
    • A61K6/0091A61K6/0023A61K6/08A61K6/083A61K6/0835A61K6/087A61K6/09C07C231/02C08L33/00C08L75/16C08L33/10C07C233/38
    • Dental composition comprising (i) a particulate filler; (ii) a polymerizable compound of the following formula (1), €ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ€ƒ AX n €ƒ€ƒ€ƒ€ƒ€ƒ(1) wherein A is a linker group containing at least n nitrogen atoms and optionally one or more acidic groups, X are moieties containing a polymerizable double bond and forming an amide bond with a nitrogen atom of A, which X may be the same or different and are represented by the following formula (2) wherein R 1 and R 2 are independent from each other and represent a hydrogen atom, a C 1-6 alkyl group or a group -(CH 2 ) m -COOM, wherein M is hydrogen atom or a metal atom, and m is an integer of from 0 to 6, L is a bond, a C 1-6 alkylene group; and n is an integer of at least 1; provided that at least one X cannot be a (meth)acryl group; and (iii) an initiator system.
    • 牙科组合物,其包含(i)颗粒状填充剂; (ii)下式(1)的可聚合化合物,其中A是连接基团(A),其中A是连接基团 基团,其含有至少n个氮原子和任选的一个或多个酸性基团,X是含有可聚合双键并与A的氮原子形成酰胺键的部分,X可以相同或不同并且由下式 (2)其中R 1和R 2彼此独立并且表示氢原子,C 1-6烷基或基团 - (CH 2)m -COOM,其中M是氢原子或金属原子,和 m是0至6的整数,L是键,C 1-6亚烷基; 并且n是至少为1的整数; 条件是至少一个X不能是(甲基)丙烯酰基; 和(iii)引发剂体系。