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1. 发明授权

US07259192B2 Molecular weight reduction of polysaccharides by electron beams 有权
标题翻译：通过电子束分子量减少多糖
公开(公告)号：US07259192B2
公开(公告)日：2007-08-21
申请号：US10606256
申请日：2003-06-24
申请人： Leo Zhaoqing Liu , Christian Priou
发明人： Leo Zhaoqing Liu , Christian Priou
IPC分类号： C08F2/46 , C09K3/32
CPC分类号： C08B37/0087 , C08B37/00 , C08B37/0033 , C08B37/0096 , C09K8/68 , C09K8/90
摘要： A method of depolymerizing galactomannan-type polysaccharide polymers and xanthan, preferably galactomannans, to a pre-selected lower molecular weight by irradiation with high energy electron beams. The preferred galactomannans for treatment according to this method are guar gum, guar splits and hydroxypropyl guar. In a preferred embodiment the guar gum is depolymerized preferably to a molecular weight of about 150,000 Daltons to about 200,000 Daltons. The depolymerized guar has a polydispersity of less than about 3.0 and is useful in oil well fracturing to enhance oil production.
摘要翻译：通过用高能电子束照射，将半乳甘露聚糖型多糖聚合物和黄原胶，优选半乳甘露聚糖解聚为预选的较低分子量的方法。根据该方法治疗的优选的半乳甘露聚糖是瓜尔胶，瓜尔胶和羟丙基瓜尔胶。在优选的实施方案中，瓜耳胶优选解聚至约150,000道尔顿至约200,000道尔顿的分子量。解聚瓜尔胶具有小于约3.0的多分散性，并且可用于油井压裂以增强油的生产。

2. 发明授权

US08889653B2 Grafting polymerization of guar and other polysaccharides by electron beams 有权
标题翻译：通过电子束将瓜尔胶和其他多糖接枝聚合
公开(公告)号：US08889653B2
公开(公告)日：2014-11-18
申请号：US12951789
申请日：2010-11-22
申请人： Leo Zhaoqing Liu , Christian Priou
发明人： Leo Zhaoqing Liu , Christian Priou
IPC分类号： A61K31/736 , C08B37/00 , A61K8/73 , C08F251/00 , A61K8/91 , A61Q19/00 , C08F251/02
CPC分类号： A61K8/91 , A61Q19/00 , C08F251/00 , C08F251/02 , C08F230/02 , C08F220/60
摘要： A method of grafting galactomannan-type polysaccharide polymers, preferably guar, to a functional group by irradiation with high energy electron beams in the presence of an unsaturated monomer-compressing the described functional group. The method may include the depolymerization of the grafted polymer to a pre-selected low molecular weight. The preferred galactomannans for treatment according to this method are guar gum, guar splits and hydroxypropyl guar. In a preferred embodiment the guar gum is also depolymerized, preferably to a molecular weight of below about 700,000 Daltons, and most preferably to a molecular weight of between about 100,000 Daltons to about 250,000 Daltons. The depolymerized guar most preferably has a polydispersity of less than about 3.0 and is useful in oil well fracturing to enhance oil production.
摘要翻译：通过在不饱和单体的存在下用高能电子束照射压缩所述官能团，将半乳甘露聚糖型多糖聚合物（优选瓜尔胶）接枝到官能团上的方法。该方法可以包括将接枝聚合物解聚成预选择的低分子量。根据该方法治疗的优选的半乳甘露聚糖是瓜尔胶，瓜尔胶和羟丙基瓜尔胶。在优选的实施方案中，瓜尔胶也被解聚，优选分子量低于约700,000道尔顿，最优选分子量为约100,000道尔顿至约250,000道尔顿。解聚瓜尔胶最好具有小于约3.0的多分散性，并且可用于油井压裂以提高产油量。

3. 发明授权

US07838667B2 Grafting polymerization of guar and other polysaccharides by electron beams 有权
标题翻译：通过电子束将瓜尔胶和其他多糖接枝聚合
公开(公告)号：US07838667B2
公开(公告)日：2010-11-23
申请号：US10607079
申请日：2003-06-25
申请人： Leo Zhaoqing Liu , Christian Priou
发明人： Leo Zhaoqing Liu , Christian Priou
IPC分类号： C08B37/00 , C07H1/08 , C08B1/00
CPC分类号： A61K8/91 , A61Q19/00 , C08F251/00 , C08F251/02 , C08F230/02 , C08F220/60
摘要： A method of grafting galactomannan-type polysaccharide polymers, preferably guar, to a functional group by irradiation with high energy electron beams in the presence of an unsaturated monomer-compressing the described functional group. The method may include the depolymerization of the grafted polymer to a pre-selected low molecular weight. The preferred galactomannans for treatment according to this method are guar gum, guar splits and hydroxypropyl guar. In a preferred embodiment the guar gum is also depolymerized, preferably to a molecular weight of below about 700,000 Daltons, and most preferably to a molecular weight of between about 100,000 Daltons to about 250,000 Daltons. The depolymerized guar most preferably has a polydispersity of less than about 3.0 and is useful in oil well fracturing to enhance oil production.
摘要翻译：通过在不饱和单体的存在下用高能电子束照射压缩所述官能团，将半乳甘露聚糖型多糖聚合物（优选瓜尔胶）接枝到官能团上的方法。该方法可以包括将接枝聚合物解聚成预选择的低分子量。根据该方法治疗的优选的半乳甘露聚糖是瓜尔胶，瓜尔胶和羟丙基瓜尔胶。在优选的实施方案中，瓜尔胶也被解聚，优选分子量低于约700,000道尔顿，最优选分子量为约100,000道尔顿至约250,000道尔顿。解聚瓜尔胶最好具有小于约3.0的多分散性，并且可用于油井压裂以提高产油量。

4. 发明授权

US08796487B2 Process for the preparation of highly purified, dialkydithiophosphinic compounds 有权
标题翻译：制备高纯度二烷基二硫代磷酸化合物的方法
公开(公告)号：US08796487B2
公开(公告)日：2014-08-05
申请号：US12455847
申请日：2009-06-08
申请人： Leo Zhaoqing Liu , Gary Woodward
发明人： Leo Zhaoqing Liu , Gary Woodward
IPC分类号： C07F9/34 , C07F9/30
CPC分类号： C07F9/34 , C07F9/301
摘要： An improved process for production of dialkyldithiophosphinic acid including sulfurizing a purified dialkylphosphinic acid by: reacting a hypophosphorous acid or salt with a stoichiometric excess of an alpha olefin in the presence of a free radical initiator to form a reaction product comprising monoalkylphosphinic acid and dialkylphosphinic acid; adding sufficient aqueous base to the reaction product to i) form the salts of the phosphinic acids, and ii) establish an aqueous phase and an organic phase, wherein a monoalkylphosphinic acid solubilizes into an aqueous phase; separating the organic phase from the aqueous phase; acidifying the organic phase and removing the olefin from the organic phase; isolating the purified dialkylphosphinic acid product; and sulfurizing the purified dialkylphosphinic acid product to form a dialkydithiophosphinic acid. The present invention also provides a process for preparing purified dialkylthiophosphinic chloride, and a process for preparing purified dialkylmonothiophosphinic acids.
摘要翻译：一种制备二烷基二硫代次膦酸的改进方法，包括通过以下方法硫化纯化的二烷基次膦酸：在自由基引发剂的存在下使次磷酸或盐与化学计量过量的α-烯烃反应形成包含单烷基次膦酸和二烷基次膦酸的反应产物; 向反应产物中加入足够的碱水溶液以i）形成次膦酸的盐，和ii）建立水相和有机相，其中单烷基次膦酸溶于水相中; 从水相中分离有机相; 酸化有机相并从有机相中除去烯烃; 分离纯化的二烷基次膦酸产物; 并将纯化的二烷基次膦酸产物硫化以形成二烷基次膦酸。本发明还提供了一种制备纯化的二烷基硫代次膦酸氯化物的方法和一种制备纯化的二烷基硫代次膦酸的方法。

5. 发明申请

US20080103330A1 Process for the preparation of highly purified, dialkydithiophosphinic compounds 有权
标题翻译：制备高纯度二烷基二硫代磷酸化合物的方法
公开(公告)号：US20080103330A1
公开(公告)日：2008-05-01
申请号：US11977620
申请日：2007-10-25
申请人： Leo Zhaoqing Liu , Gary Woodward
发明人： Leo Zhaoqing Liu , Gary Woodward
IPC分类号： C07F9/30 , C07F9/34
CPC分类号： C07F9/34 , C07F9/301
摘要： An improved process for production of dialkyldithiophosphinic acid including sulfurizing a purified dialkylphosphinic acid by: reacting a hypophosphorous acid or salt with a stoichiometric excess of an alpha olefin in the presence of a free radical initiator to form a reaction product comprising monoalkylphosphinic acid and dialkylphosphinic acid; adding sufficient aqueous base to the reaction product to i) form the salts of the phosphinic acids, and ii) establish an aqueous phase and an organic phase, wherein a monoalkylphosphinic acid solubilizes into an aqueous phase; separating the organic phase from the aqueous phase; acidifying the organic phase and removing the olefin from the organic phase; isolating the purified dialkylphosphinic acid product; and sulfurizing the purified dialkylphosphinic acid product to form a dialkydithiophosphinic acid. The present invention also provides a process for preparing purified dialkylthiophosphinic chloride, and a process for preparing purified dialkylmonothiophosphinic acids.
摘要翻译：一种制备二烷基二硫代次膦酸的改进方法，包括通过以下方法硫化纯化的二烷基次膦酸：在自由基引发剂的存在下使次磷酸或盐与化学计量过量的α-烯烃反应，形成包含单烷基次膦酸和二烷基次膦酸的反应产物; 向反应产物中加入足够的碱水溶液以i）形成次膦酸的盐，和ii）建立水相和有机相，其中单烷基次膦酸溶于水相中; 从水相中分离有机相; 酸化有机相并从有机相中除去烯烃; 分离纯化的二烷基次膦酸产物; 并将纯化的二烷基次膦酸产物硫化以形成二烷基次膦酸。本发明还提供了一种制备纯化的二烷基硫代次膦酸氯化物的方法和一种制备纯化的二烷基硫代次膦酸的方法。

6. 发明授权

US07030275B2 Monomer compound comprising several cationic groups, process for making the same, and polymers comprising units deriving therefrom 失效
公开(公告)号：US07030275B2
公开(公告)日：2006-04-18
申请号：US10453240
申请日：2003-06-03
申请人： Leo Zhaoqing Liu
发明人： Leo Zhaoqing Liu
IPC分类号： C07C213/00
CPC分类号： C08F20/60 , C07C237/10 , C08F20/34 , C11D3/3769
摘要： Monomer compounds comprising several cationic groups, a process for making such compounds and polymers derived from such compounds are provided. The monomer compounds are according to formula (I): wherein R1 is a hydrogen atom, a methyl group or an ethyl group, A, which is identical or different, is a group comprising an ester group of formula —A1—C(O)—O—A2—, or an amide group of formula —A1—C(O)—NR10—A2—, wherein: R10, which is identical or different, is hydrogen or an alkyl, hydroxyalkyl, or aminoalkyl C1–C6 linear or branched group, A1, which is identical or different is a covalent bond or a group of formula —(CH2)p1— wherein p1 is an integer of from 1 to 6, A2, which is identical or different, is a linear or branched hydrocarbon group comprising optionally N, O, or S heteroatoms or heterogroups, optionally substituted, optionally forming or comprising a cycle, R1, R2, R3, R4, R5 and R6, which are identical or different, are hydrogen, alkyl, hydroxyalkyl, or aminoalkyl C1–C6 linear or branched groups, or, if inside the brackets, form a heterocycle with group A2, m is an integer of from 1 to 10, n is an integer of from 1 to 6, Z is —O', —C(O)O—, or —C(O)NH—, B is a linear or branched C2–C12 polymethylene chain, optionally comprising heteroatoms or heterogroups and optionally substituted with one or several hydroxy or amino groups, and X−, which are identical or different, are counter ions.

7. 发明授权

US06376631B1 Processes to control the residual monomer level of copolymers of tertiary amino monomer with a vinyl-functional monomer 有权
标题翻译：控制叔氨基单体与乙烯基官能单体的共聚物残留单体含量的方法
公开(公告)号：US06376631B1
公开(公告)日：2002-04-23
申请号：US09670570
申请日：2000-09-27
申请人： Dominic Wai Kwing Yeung , Leo Zhaoqing Liu , Richard E. Rice
发明人： Dominic Wai Kwing Yeung , Leo Zhaoqing Liu , Richard E. Rice
IPC分类号： C08F12606
CPC分类号： C08F220/34 , C08F2220/281 , C08F220/06
摘要： The present invention relates to processes for making polymers from at least one tertiary amino-containing monomer and at least one vinyl-functional monomer, while controlling residual monomers and avoiding production of Michael addition adducts. The process employs one or more of the following steps to avoid such adducts, maintaining at least one tertiary amino-containing monomer and at least one vinyl-functional monomer separate until the polymerization reaction, maintaining the at least one tertiary amino-containing monomer and at least one vinyl-functional monomer free of water until the polymerization reaction, and employing high temperatures for the polymerization reaction. The polymers are useful in personal care products, fabric detergent, hand dishwashing detergent, oil well treating chemicals, fire-fighting foam, agricultural chemicals, flocculants, coagulants, and household cleaners.
摘要翻译：本发明涉及从至少一种含叔氨基的单体和至少一种乙烯基官能单体制备聚合物的方法，同时控制残余单体并避免生产迈克尔加成加合物。该方法采用一个或多个以下步骤来避免这种加合物，保持至少一种含叔氨基的单体和至少一种乙烯基官能单体直到聚合反应，保持至少一种含叔氨基的单体并保持在至少一种乙烯基官能单体不含水直到聚合反应，并且使用高温进行聚合反应。聚合物可用于个人护理产品，织物洗涤剂，洗手液洗涤剂，油井处理化学品，消防泡沫，农药，絮凝剂，凝结剂和家用清洁剂。

8. 发明授权

US08258342B2 Process for making a (meth)acrylamide monomer 有权
标题翻译：制备（甲基）丙烯酰胺单体的方法
公开(公告)号：US08258342B2
公开(公告)日：2012-09-04
申请号：US12077384
申请日：2008-03-19
申请人： Leo Zhaoqing Liu
发明人： Leo Zhaoqing Liu
IPC分类号： C07C231/02
CPC分类号： C07C231/02 , C07C213/06 , C07C219/08 , C07C233/36
摘要： A method for making a (meth)acrylamide monomer, comprises reacting a (meth)acrylate ester with an amino-functional compound in an organic solvent in the presence of a transesterification catalyst.
摘要翻译：一种制备（甲基）丙烯酰胺单体的方法，包括在酯交换催化剂存在下，使有机溶剂中的（甲基）丙烯酸酯与氨基官能化合物反应。

9. 发明申请

US20090253931A1 Process for the preparation of highly purified, dialkydithiophosphinic compounds 有权
标题翻译：制备高纯度二烷基二硫代磷酸化合物的方法
公开(公告)号：US20090253931A1
公开(公告)日：2009-10-08
申请号：US12455847
申请日：2009-06-08
申请人： Leo Zhaoqing Liu , Gary Woodward
发明人： Leo Zhaoqing Liu , Gary Woodward
IPC分类号： C07F9/30
CPC分类号： C07F9/34 , C07F9/301
摘要： An improved process for production of dialkyldithiophosphinic acid including sulfurizing a purified dialkylphosphinic acid by: reacting a hypophosphorous acid or salt with a stoichiometric excess of an alpha olefin in the presence of a free radical initiator to form a reaction product comprising monoalkylphosphinic acid and dialkylphosphinic acid; adding sufficient aqueous base to the reaction product to i) form the salts of the phosphinic acids, and ii) establish an aqueous phase and an organic phase, wherein a monoalkylphosphinic acid solubilizes into an aqueous phase; separating the organic phase from the aqueous phase; acidifying the organic phase and removing the olefin from the organic phase; isolating the purified dialkylphosphinic acid product; and sulfurizing the purified dialkylphosphinic acid product to form a dialkyldithiophosphinic acid. The present invention also provides a process for preparing purified dialkylthiophosphinic chloride, and a process for preparing purified dialkylmonothiophosphinic acids.
摘要翻译：一种制备二烷基二硫代次膦酸的改进方法，包括通过以下方法硫化纯化的二烷基次膦酸：在自由基引发剂的存在下使次磷酸或盐与化学计量过量的α-烯烃反应，形成包含单烷基次膦酸和二烷基次膦酸的反应产物; 向反应产物中加入足够的碱水溶液以i）形成次膦酸的盐，和ii）建立水相和有机相，其中单烷基次膦酸溶于水相中; 从水相中分离有机相; 酸化有机相并从有机相中除去烯烃; 分离纯化的二烷基次膦酸产物; 并将纯化的二烷基次膦酸产物硫化以形成二烷基二硫代次膦酸。本发明还提供了一种制备纯化的二烷基硫代次膦酸氯化物的方法和一种制备纯化的二烷基硫代次膦酸的方法。

10. 发明授权

US07247693B2 Monomer compound comprising several cationic groups, process for making the same, and polymers comprising units deriving therefrom 有权
公开(公告)号：US07247693B2
公开(公告)日：2007-07-24
申请号：US11327014
申请日：2006-01-06
申请人： Leo Zhaoqing Liu , Dominic Wai-Kwing Yeung
发明人： Leo Zhaoqing Liu , Dominic Wai-Kwing Yeung
IPC分类号： C08F20/56 , C08F20/60
CPC分类号： C08F20/60 , C07C237/10 , C08F20/34 , C11D3/3769
摘要： A polymer includes repetitive units derived from a monomer compound according to formula (I): wherein R1 is a hydrogen atom, a methyl group or an ethyl group, A, which is identical or different, is a group comprising an ester group of formula -A1-C(O)—O-A2-, or an amide group of formula -A1-C(O)—NR10-A2-, wherein: R10, which is identical or different, is hydrogen or an alkyl, hydroxyalkyl, or aminoalkyl C1-C6 linear or branched group, A1, which is identical or different is a covalent bond or a group of formula —(CH2)p1— wherein p1 is an integer of from 1 to 6, A2, which is identical or different, is a linear or branched hydrocarbon group comprising optionally N, O, or S heteroatoms or heterogroups, optionally substituted, optionally forming or comprising a cycle, R1, R2, R3, R5 and R6, which are identical or different, are hydrogen, alkyl, hydroxyalkyl, or aminoalkyl C1-C6 linear or branched groups, or, if inside the brackets, form a heterocycle with group A2, m is an integer of from 1 to 10, n is an integer of from 1 to 6, Z is —O—, —C(O)O—, or —C(O)NH—, B is a linear or branched C2-C12 polymethylene chain, optionally comprising heteroatoms or heterogroups, and optionally substituted with one or several hydroxy or amino groups, and X−, which are identical or different, are counter ions.

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