公开(公告)号：US20120015201A1

公开(公告)日：2012-01-19

申请号：US13202911

申请日：2010-02-19

Applicant: Helmut Zecha ,  Gerhard Kögler

Inventor： Helmut Zecha ,  Gerhard Kögler

IPC: B32B27/06 ,  B32B27/08 ,  C09J131/04 ,  C08F218/08 ,  C08F2/00

CPC classification number: C08F218/08 ,  C08F2/001 ,  C08F2/24 ,  C08F2/30 ,  C09J123/0853 ,  Y10T428/31855 ,  Y10T428/3188 ,  C08F210/02

Abstract: The invention provides a process for preparing vinyl acetate-ethylene copolymers by means of free-radically initiated emulsion polymerization of vinyl acetate and 18% to 34% by weight of ethylene, based on the total weight of the vinyl acetate and ethylene monomers, and, optionally, further comonomers, characterized in that polymerization takes place in the presence of at least one protective colloid and of 0.5% to 4% by weight, based on the total amount of monomers, of at least one nonionic, ethoxylated emulsifier with a branched or linear alkyl radical or in the form of ethylene oxide-propylene oxide copolymers, and in the absence of chain transfer agent, and, before the initiation of the polymerization, 10% to 70% by weight of the vinyl acetate monomer and 40% to 100% by weight of the ethylene monomer are included in the initial charge, up to 100% by weight of the protective colloid fraction is included in the initial charge, at least 25% by weight of the emulsifier fraction is included in the initial charge, and the remaining fractions of monomers, protective colloid and emulsifier are metered in during the polymerization, the procedure being such that the criterion of process COP meets the condition 2.5≦COP≦70, where COP=100×(ETM2.5×ETV1.25×EA2.5×EV1.5×VV−1), where ETM=MEt/MM, ETV=MEtV/MEt, EA=100 ME/MM, EV=MEV/ME and VV=MVacV/MVac, where MEt=total mass of ethylene in kg, MM=total mass of monomer in kg, MEtV=mass of ethylene charge in kg, ME=total mass of emulsifier in kg, MEV=mass of emulsifier charge in kg; MVacV=mass of vinyl acetate charge in kg, and MVac=total mass of vinyl acetate in kg.

Abstract translation: 本发明提供了一种通过乙酸乙烯酯的自由基引发的乳液聚合和基于乙酸乙烯酯和乙烯单体的总重量的18至34重量％的乙烯制备乙酸乙烯酯 - 乙烯共聚物的方法， 任选的另外的共聚单体，其特征在于聚合在至少一种保护胶体存在下进行，并且基于单体总量为0.5重量％至4重量％的至少一种非离子，乙氧基化乳化剂与支链或 直链烷基或环氧乙烷 - 环氧丙烷共聚物的形式，并且在不存在链转移剂的情况下，并且在聚合开始之前，10重量％至70重量％的乙酸乙烯酯单体和40重量％至100重量％ 在初始充电中包括乙烯单体的重量百分比，最初至少100重量％的保护胶体部分包括在初始充电中，至少25重量％的乳化剂组分包括 在初始充电中，在聚合过程中计量单体，保护胶体和乳化剂的剩余部分，程序使得方法COP的标准满足条件2.5＆lt; COP＆nlE; 70，其中COP = 100×（ ETM2.5×ETV1.25×EA2.5×EV1.5×VV-1），其中ETM = MEt / MM，ETV = MEtV / MEt，EA = 100ME / MM，EV = MEV / ME，VV = MVacV / MVac，其中MEt =以kg为单位的乙烯总质量，MM =单位总质量（kg），MEtV =乙烯装料量（kg），ME =乳化剂总质量（kg），MEV =乳化剂装料量（kg） MVacV =乙酸乙烯酯的质量（kg），MVac =乙酸乙烯酯的总质量（kg）。

公开(公告)号：US06794466B2

公开(公告)日：2004-09-21

申请号：US10035373

申请日：2001-10-19

Applicant: Helmut Zecha ,  Rudolf Weissgerber ,  Francis Petrocelli

Inventor： Helmut Zecha ,  Rudolf Weissgerber ,  Francis Petrocelli

IPC: C08F238

CPC classification number: C08F18/08

Abstract: The present invention elates to a vinyl acetate based polymer latex composition obtained by emulsion polymerization of: (a) polyvinyl alcohol, (c) a monomer mixture comprising vinyl acetate, and (d) optionally one or more additional co-monomer(s), in presence of (c) 0.0001-0.05 wt. % of a chain transfer agent, based on total monomer weight, said vinyl acetate based polymer latex composition having a weight average particle size ≧400 nm and a higher shear thinning factor than the vinyl acetate based polymer latex composition (a), (b) and (d) obtained in the absence of the chain transfer agent (c). According to one embodiment, emulsion polymerization is carried out in presence of 0.001 to 0.05 wt. % of a chain transfer agent selected from the group consisting of aldehydes and chain transfer agents having a similar chain transfer constant with regard to vinyl acetate as the monomer. According to another embodiment, emulsion polymerization is carried out in presence of 0.0001 to 0.01 wt. % of a chain transfer agent selected from the group consisting of thiols, mercapto acids, and chain transfer agents having a similar chain transfer constant with regard to vinyl acetate as the monomer. The invention also relates to an adhesive comprising said vinyl acetate based polymer latex composition. Such adhesive is preferably used in paper and packaging applications or as a wood working adhesive or wood glue. The invention further relates to a process of manufacture of a vinyl acetate based polymer latex composition having a weight average particle size >400 nm, including emulsion polymerization of vinyl acetate in the presence of polyvinyl alcohol, optionally together with one or more additional co-monomer(s), wherein the emulsion polymerization is carried out in the presence of 0.0001 wt. % to 0.05 wt. % chain transfer agent, based on total monomer weight.

公开(公告)号：US08586686B2

公开(公告)日：2013-11-19

申请号：US13202911

申请日：2010-02-19

Applicant: Helmut Zecha ,  Gerhard Kögler

Inventor： Helmut Zecha ,  Gerhard Kögler

IPC: C08F218/08

CPC classification number: C08F218/08 ,  C08F2/001 ,  C08F2/24 ,  C08F2/30 ,  C09J123/0853 ,  Y10T428/31855 ,  Y10T428/3188 ,  C08F210/02

Abstract: A process for preparing a vinyl acetate-ethylene copolymer by means of free-radically initiated emulsion polymerization of vinyl acetate and ethylene and, optionally, further comonomers, performed in the presence of at least one protective colloid and at least one nonionic, ethoxylated emulsifier with an alkyl radical or at least one ethylene oxide-propylene oxide copolymer, and in the absence of chain transfer agent, and, before the initiation of the polymerization, 10% to 70% by weight of the vinyl acetate monomer and 40% to 100% by weight of the ethylene monomer are included in the initial charge, up to 100% by weight of the protective colloid fraction is included in the initial charge, at least 25% by weight of the emulsifier fraction is included in the initial charge, and the remaining fractions of monomers, protective colloid and emulsifier are metered in during the polymerization. A defined criterion of process COP is met.

Abstract translation: 通过在至少一种保护胶体和至少一种非离子的乙氧基化乳化剂的存在下，通过乙酸乙烯酯和乙烯以及任选的其它共聚单体的自由引发的乳液聚合制备乙酸乙烯酯 - 乙烯共聚物的方法， 烷基或至少一种环氧乙烷 - 环氧丙烷共聚物，并且在不存在链转移剂的情况下，在聚合开始之前，10重量％至70重量％的乙酸乙烯酯单体和40重量％至100重量％ 在初始电荷中包含乙烯单体的重量百分比，初始电荷中包含至多100重量％的保护胶体部分，初始电荷中包含至少25重量％的乳化剂部分， 在聚合期间计量单体的剩余部分，保护胶体和乳化剂。 确定过程COP的确定标准。

公开(公告)号：US20130131261A1

公开(公告)日：2013-05-23

申请号：US13813863

申请日：2011-07-25

Applicant: Helmut Zecha ,  Gerhard Kögler

Inventor： Helmut Zecha ,  Gerhard Kögler

IPC: C08F2/06

CPC classification number: C08F2/06 ,  C08F2/26 ,  C08F210/02 ,  C08F218/08

Abstract: The invention provides processes for preparing vinyl acetate-ethylene copolymers by means of free-radical initiated emulsion polymerization of vinyl acetate, ethylene and optionally one or more further comonomers in the presence of at least one protective colloid and optionally at least one emulsifier, characterized in that the vinyl acetate-ethylene copolymers contain 18 to 45% by weight of ethylene units, based on the total weight of the vinyl acetate-ethylene copolymers, and at least 70% by weight of ethylene units, based on the total weight of the ethylene units and of the further comonomer units of the vinyl acetate-ethylene copolymers, and the free-radical initiated emulsion polymerization is performed in the presence of A) 0.5 to 20% by weight, based on the total weight of the monomers used overall, of one or more solvents, or B) 0.1 to 20% by weight, based on the total weight of monomers used overall, of one or more solvents, and 0.5 to 4% by weight, based on the total weight of monomers used overall, of one or more anionic sulphosuccinic esters of the general formula R1O—CO—CH2—CH (SO3M)—CO—O—R1 (I) in which M is a cation, R1 is a linear or branched alkyl radical having 4 to 17 carbon atoms, an alkylene oxide group —(R2—O)n-X or a cation M, where R2 is a linear or branched alkylene unit having 2 to 5 carbon atoms, n is an integer from 2 to 20 and X is a linear or branched alkyl radical having 4 to 17 carbon atoms, where at most one R1 radical in the general formula (I) is a cation M.

Abstract translation: 本发明提供了在至少一种保护胶体和任选的至少一种乳化剂的存在下，通过乙酸乙烯酯，乙烯和任选的一种或多种另外的共聚单体的自由基引发的乳液聚合制备乙酸乙烯酯 - 乙烯共聚物的方法，其特征在于 乙酸乙烯酯 - 乙烯共聚物含有18至45重量％的乙烯单元，基于乙酸乙烯酯 - 乙烯共聚物的总重量，至少70重量％的乙烯单元，基于乙烯的总重量 单元和乙酸乙烯酯 - 乙烯共聚物的另外的共聚单体单元和自由基引发的乳液聚合在A = 0.5-20重量％的存在下进行，基于总体使用的单体的总重量， 一种或多种溶剂，或B）基于总体使用的单体总重量为0.1至20重量％的一种或多种溶剂，和基于总重量的0.5至4重量％ f单体，其中M是阳离子的一种或多种通式为R 1 O-CO-CH 2 -CH（SO 3 M）-CO-O-R 1（I）的阴离子磺基琥珀酸酯，R 1是直链或支链烷基 具有4至17个碳原子，环氧烷基 - （R2-O）nX或阳离子M，其中R2是具有2至5个碳原子的直链或支链亚烷基单元，n是2至20的整数，X是 具有4至17个碳原子的直链或支链烷基，其中通式（I）中至多一个R 1基团是阳离子M.

公开(公告)号：US20070088120A1

公开(公告)日：2007-04-19

申请号：US11254099

申请日：2005-10-19

Applicant: Helmut Zecha ,  Holger Kuenstle

Inventor： Helmut Zecha ,  Holger Kuenstle

IPC: C08L31/00

CPC classification number: C08F263/02 ,  C08F210/02 ,  C08F218/10 ,  C08F218/18 ,  C08F220/18 ,  C08F220/58 ,  C08F228/02 ,  C08F255/02 ,  C08F291/00 ,  C08L51/003 ,  C09D151/003 ,  C08L2666/02

Abstract: The present invention relates to a vinyl ester based polymer latex composition obtainable by free radical emulsion polymerization in substantial absence of a protective colloid and in the presence of no or small amounts of a surfactant, and to a process of making the same. The invention further pertains to a dispersion incorporating said vinyl ester based polymer latex composition, products comprising said dispersion, and various uses of the dispersion.

Abstract translation: 本发明涉及一种基本上不存在保护胶体并且在不存在或少量表面活性剂的情况下通过自由基乳液聚合获得的乙烯基酯基聚合物胶乳组合物及其制备方法。 本发明还涉及包含所述基于乙烯基酯的聚合物胶乳组合物，包含所述分散体的产品和分散体的各种用途的分散体。

公开(公告)号：US07649067B2

公开(公告)日：2010-01-19

申请号：US11254099

申请日：2005-10-19

Applicant: Helmut Zecha ,  Holger Kuenstle

Inventor： Helmut Zecha ,  Holger Kuenstle

IPC: C08F255/02 ,  C08F263/02 ,  C08F291/00 ,  C08L51/00

CPC classification number: C08F263/02 ,  C08F210/02 ,  C08F218/10 ,  C08F218/18 ,  C08F220/18 ,  C08F220/58 ,  C08F228/02 ,  C08F255/02 ,  C08F291/00 ,  C08L51/003 ,  C09D151/003 ,  C08L2666/02

Abstract: The present invention relates to a vinyl ester based polymer latex composition obtainable by free radical emulsion polymerization in substantial absence of a protective colloid and in the presence of no or small amounts of a surfactant, and to a process of making the same. The invention further pertains to a dispersion incorporating said vinyl ester based polymer latex composition, products comprising said dispersion, and various uses of the dispersion.

Abstract translation: 本发明涉及一种基本上不存在保护胶体并且在不存在或少量表面活性剂的情况下通过自由基乳液聚合获得的乙烯基酯基聚合物胶乳组合物及其制备方法。 本发明还涉及包含所述基于乙烯基酯的聚合物胶乳组合物，包含所述分散体的产品和分散体的各种用途的分散体。

公开(公告)号：US06552115B1

公开(公告)日：2003-04-22

申请号：US09690422

申请日：2000-10-17

Applicant: Helmut Zecha ,  Rudolf Weissgerber ,  Frank Geiger

Inventor： Helmut Zecha ,  Rudolf Weissgerber ,  Frank Geiger

IPC: C08F216

CPC classification number: C08F218/04 ,  C08F261/04

Abstract: The present invention relates to a vinyl acetate based polymer latex composition obtained by emulsion polymerization, the polymer comprising PVOH, and a monomer mixture, said monomer mixture comprising vinyl acetate, and a pre-crosslinking monomer selected from one or more polyethylenically unsaturated compounds wherein said pre-crosslinking monomer is present in amount of less than 0.01% by weight based on the total monomer content and which pre-crosslinking monomer is initially charged to the polymerization reaction mixture. The invention further relates to use of the vinyl acetate based polymer latex in an adhesive, preferably a woodworking adhesive and to an adhesive, preferably a woodworking adhesive comprising said latex.

Abstract translation: 本发明涉及通过乳液聚合获得的乙酸乙烯酯基聚合物胶乳组合物，包含PVOH的聚合物和单体混合物，所述单体混合物包含乙酸乙烯酯和选自一种或多种多烯属不饱和化合物的预交联单体，其中所述 预交联单体的存在量小于基于单体总量的0.01重量％，并且哪些预交联单体最初加入到聚合反应混合物中。 本发明还涉及在粘合剂，优选木工粘合剂和粘合剂，优选包含所述胶乳的木工粘合剂中使用乙酸乙烯酯基聚合物胶乳。