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1. 发明授权

US06303712B1 Process for producing vinyl chloride polymer 失效
标题翻译：制备氯乙烯聚合物的方法
公开(公告)号：US06303712B1
公开(公告)日：2001-10-16
申请号：US09377917
申请日：1999-08-20
申请人： Kazuhiro Kumakura , Makoto Ooura , Tadashi Amano
发明人： Kazuhiro Kumakura , Makoto Ooura , Tadashi Amano
IPC分类号： C08F218
CPC分类号： C08F14/06 , C08F2/18
摘要： In a process for producing a vinyl chloride polymer by suspension polymerization in a polymerization vessel having a coating film of a polymer scale preventive agent on the polymerization vessel inner wall and other inner surfaces, the polymerization is initiated by introducing an oil-soluble polymerization initiator having 10-hour half-life temperature of from 30° C. to 55° C., at a particular position of the interior of the liquid phase of polymerization materials charged. The position satisfys the following expression: H≦0.7H0 wherein H represents a height from the bottom of the polymerization vessel to the position where the polymerization initiator is introduced, and H0 represents a height from the bottom of the polymerization vessel to the liquid surface of the liquid phase. This process can effectively prevent polymer scales from adhering to the polymerization vessel inner wall of course and also to the baffle on its side facing the polymerization vessel inner wall at the gas/liquid interface and the vicinity thereof even with repetition of polymerization of vinyl chloride. Good formed products with less fish eyes can be obtained.
摘要翻译：在聚合容器内壁等内表面具有聚合物防垢剂的涂膜的聚合容器中通过悬浮聚合制造氯乙烯聚合物的方法中，通过引入具有在10℃的半衰期温度为30℃至55℃，在聚合物质液相内部的特定位置带电。该位置满足以下表达式：其中H表示从聚合容器的底部到引入聚合引发剂的位置的高度，H0表示从聚合容器的底部到液相的液面的高度。该方法可以有效地防止聚合物垢在当然的情况下粘附到聚合容器的内壁上，并且还可以在气/液界面及其附近面向聚合容器内壁的侧面上，甚至重复聚合氯乙烯。可以获得鱼眼少的良好成型产品。

2. 发明授权

US07001960B2 Process for producing vinyl chloride-based polymer 有权
标题翻译：生产氯乙烯基聚合物的方法
公开(公告)号：US07001960B2
公开(公告)日：2006-02-21
申请号：US11067717
申请日：2005-03-01
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08F2/20
CPC分类号： C08F114/06
摘要： A process for producing a vinyl chloride-based polymer by suspension polymerization is provided. The polymerization is initiated in the presence of (A) a particular hydroxypropylmethylcellulose, (B) a particular partially saponified PVA with a saponification degree of 75 to 85 mol % and an average polymerization degree of 1000 to 3000, and (C) a particular partially saponified PVA with a saponification degree of 20 to 57 mol % and an average polymerization degree of 150 to 600 in a specified ration, and said (C) is also additionally added to the polymerization system when a conversion rate is 15–50%. Polymers with a high porosity, excellent plasticizer absorption, extremely low levels of fish eyes, and a high bulk specific gravity are produced at a high level of productivity.
摘要翻译：提供了一种通过悬浮聚合制备氯乙烯基聚合物的方法。在（A）特定的羟丙基甲基纤维素，（B）皂化度为75至85摩尔％，平均聚合度为1000至3000的特定部分皂化的PVA的存在下引发聚合，和（C）特定部分在规定的比例中皂化度为20〜57摩尔％，平均聚合度为150〜600的皂化PVA，当转化率为15〜50％时，也加入到聚合体系中。以高生产率生产具有高孔隙率，优异的增塑剂吸收性，极高水平的鱼眼和高体积比重的聚合物。

3. 发明授权

US06861488B2 Process for producing a vinyl chloride-based polymer 失效
标题翻译：氯乙烯系聚合物的制造方法
公开(公告)号：US06861488B2
公开(公告)日：2005-03-01
申请号：US10642172
申请日：2003-08-18
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08F2/18 , C08F14/06 , C08F14/08 , C08F4/28
CPC分类号： C08F14/06 , C08F2/18 , C08F14/08 , C08F2/16
摘要： There is provided a process for producing a vinyl chloride-based polymer by conducting a suspension polymerization in an aqueous medium using an oil soluble polymerization initiator, wherein the oil soluble polymerization initiator utilizes a combination of (A) t-amyl peroxyneodecanoate and (B) a peroxide-based polymerization initiator with a 10 hour half-life temperature in a solution with a concentration of 0.1 mol/liter in trichloroethylene within a range of at least 30° C. but less than 55° C., and when a predetermined polymerization conversion rate is reached, the polymerization reaction temperature is raised by a predetermined amount, followed by addition of an antioxidant to said polymerization mixture to halt the polymerization reaction. According to this process, a vinyl chloride-based polymer with good anti-initial discoloration can be produced in high yield and with good productivity.
摘要翻译：提供了一种通过使用油溶性聚合引发剂在水性介质中进行悬浮聚合来制备氯乙烯类聚合物的方法，其中油溶性聚合引发剂利用（A）过氧新癸酸叔戊酯和（B）在三氯乙烯浓度为0.1摩尔/升的溶液中，在至少30℃但小于55℃的范围内具有10小时半衰期温度的过氧化物基聚合引发剂，当预定的聚合使聚合反应温度升高预定量，然后向所述聚合混合物中加入抗氧化剂以停止聚合反应。根据该方法，可以高产率和高生产率制备具有良好抗初始变色性的氯乙烯系聚合物。

4. 发明授权

US07112637B2 Process for producing vinyl chloride polymer 有权
标题翻译：制备氯乙烯聚合物的方法
公开(公告)号：US07112637B2
公开(公告)日：2006-09-26
申请号：US10561962
申请日：2004-12-21
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08F2/18 , C08F14/06
CPC分类号： C08F14/06 , C08F2/18
摘要： There is provided a process for producing a vinyl chloride-based polymer, in which a suspension polymerization of either vinyl chloride monomer, or a mixture of vinyl chloride monomer and another copolymerizable monomer, is conducted in a polymerization vessel fitted with a reflux condenser, the process including the steps of: (A) adding to the reaction mixture a high-activity, oil-soluble polymerization initiator, with a 10-hour half life temperature of no more than 40° C. at a concentration of 0.1 mol/L in benzene, for a specified time within a period from the commencement of heat removal using the reflux condenser through to completion of the polymerization, (B) adding water either continuously or intermittently to the reaction mixture through the supply pipe for the polymerization initiator, at least during the period from the commencement of addition of the high-activity, oil-soluble polymerization initiator through to completion of that addition, and (C) passing steam through the supply pipe following completion of the addition of the water. According to the present invention, the process for producing a vinyl chloride-based polymer by aqueous suspension polymerization in a polymerization vessel fitted with a reflux condenser can be improved, the heat removal capability can be utilized effectively to shorten the polymerization time, and a high quality vinyl chloride-based polymer with an extremely low level of fish eyes can be produced.
摘要翻译：提供了一种氯乙烯系聚合物的制造方法，其中氯乙烯单体或氯乙烯单体与其它可共聚单体的混合物的悬浮聚合在配有回流冷凝器的聚合容器中进行，方法包括以下步骤：（A）将浓度为0.1mol / L的10分钟半衰期不大于40℃的高活性油溶性聚合引发剂加入到反应混合物中苯，在使用回流冷凝器进行除热开始到完成聚合之前的一段时间内，（B）通过聚合引发剂的供给管连续地或间歇地向反应混合物中加入水，至少在从开始加入高活性油溶性聚合引发剂到完成该添加的期间，和（C）使蒸汽通过th e在完成添加水后供应管道。根据本发明，通过在配有回流冷凝器的聚合容器中通过水悬浮聚合制造氯乙烯类聚合物的方法可以得到改善，可以有效地利用除热能力来缩短聚合时间，并且高可以生产具有极低水平鱼眼的优质氯乙烯基聚合物。

5. 发明申请

US20080176995A1 DISPERSION STABILIZER FOR SUSPENSION POLYMERIZATION AND METHOD OF PRODUCING VINYL CHLORIDE-BASED POLYMER USING SAME 审中-公开
标题翻译：用于悬浮聚合的分散稳定剂及使用其制备基于氯乙烯的聚合物的方法
公开(公告)号：US20080176995A1
公开(公告)日：2008-07-24
申请号：US12017869
申请日：2008-01-22
申请人： Makoto OOURA , Tadashi Amano , Minoru Shigemitsu , Shingo Niinobe
发明人： Makoto OOURA , Tadashi Amano , Minoru Shigemitsu , Shingo Niinobe
IPC分类号： C09K3/00 , C08L27/06
CPC分类号： C08F14/06 , C08L1/284 , C08L27/06 , C08F2/20 , C08L2666/26
摘要： Provided is a dispersion stabilizer for suspension polymerization that contains a hydroxypropylmethylcellulose with a degree of methoxy group substitution of 27 to 30% by mass and a degree of hydroxypropoxy group substitution of 5 to 12% by mass, in which the viscosity at 20° C. of a 2% by mass aqueous solution of the hydroxypropylmethylcellulose is within a range from 5 to 1,600 mPa·s, and in 2 ml of a 0.2% by mass solution of the hydroxypropylmethylcellulose, the number of undissolved fibers with a particle size within a range from 8 to 200 μm, as measured by a Coulter counter method, is not more than 1,000, and the number of undissolved fibers with a particle size of 50 μm or greater measured using the same method is not more than 20. By employing a method of producing a vinyl chloride-based polymer that uses this dispersion stabilizer, a vinyl chloride-based polymer with extremely low levels of fish eyes and defects derived from foreign objects can be produced.
摘要翻译：提供一种悬浮聚合用分散稳定剂，其含有甲氧基取代度为27〜30质量％，羟基丙氧基取代度为5〜12质量％的羟丙基甲基纤维素，其中20℃下的粘度的羟丙基甲基纤维素的2质量％水溶液在5〜1600mPa.s的范围内，在2ml的0.2质量％羟丙基甲基纤维素溶液中，粒径在一定范围内的未溶解纤维的数量通过Coulter反方法测量的8至200μm的不超过1,000个，使用相同方法测量的粒径为50μm或更大的未溶解纤维的数量不超过20.通过采用方法制造使用该分散稳定剂的基于氯乙烯的聚合物，可以制造具有极低水平鱼眼的氯乙烯类聚合物和由异物衍生的缺陷。

6. 发明申请

US20070100098A1 Process for producing vinyl chloride polymer 有权
公开(公告)号：US20070100098A1
公开(公告)日：2007-05-03
申请号：US10561909
申请日：2004-12-21
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08F4/28
CPC分类号： C08F14/06 , C08F2/18
摘要： There is provided a process for producing a vinyl chloride-based polymer, in which a suspension polymerization of either vinyl chloride monomer, or a mixture of vinyl chloride monomer and another copolymerizable monomer, is conducted in a polymerization vessel fitted with a reflux condenser, the process including the steps of: (A) adding to the reaction mixture a high-activity, oil-soluble polymerization initiator, with a 10-hour half life temperature of no more than 40° C. at a concentration of 0.1 mol/L in benzene, for a specified time within a period from the commencement of heat removal using the reflux condenser through to completion of the polymerization, and (B) adding an antioxidant either continuously or intermittently to the reaction mixture at least during the period from the commencement of addition of the high-activity, oil-soluble polymerization initiator through to completion of that addition. According to the present invention, the process for producing a vinyl chloride-based polymer by aqueous suspension polymerization in a polymerization vessel fitted with a reflux condenser can be improved, the heat removal capability can be utilized effectively to shorten the polymerization time, and a high quality vinyl chloride-based polymer with an extremely low level of fish eyes can be produced.

7. 发明授权

US06433074B1 Process for producing vinyl chloride polymer 失效
标题翻译：制备氯乙烯聚合物的方法
公开(公告)号：US06433074B1
公开(公告)日：2002-08-13
申请号：US09634638
申请日：2000-08-08
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08K513
CPC分类号： C08K5/13 , C08F14/06 , C08K5/372 , C08F2/44 , C08L27/06
摘要： Provided is a vinyl chloride polymer production process comprising the steps of polymerizing in an aqueous medium a vinyl chloride monomer alone or a mixture of monomers including the vinyl chloride monomer, and adding an antioxidant to starting materials or a polymerization reaction mixture. As the antioxidant, a mixed antioxidant comprised of an antioxidant A which is liquid at 20° C. and an antioxidant B which is powdery at 20° C. is used. This process is well operable, enables polymerization to be sufficiently terminated using an antioxidant in a small quantity and enables production of vinyl chloride polymers having less uneven plasticizer absorption and having both good anti-initial-discoloration properties and good thermal stability.
摘要翻译：提供了一种氯乙烯聚合物制备方法，其包括以下步骤：在水性介质中聚合单独的氯乙烯单体或包含氯乙烯单体的单体混合物，并向原料或聚合反应混合物中加入抗氧化剂。作为抗氧化剂，使用由20℃下为液体的抗氧化剂A和20℃下粉末状的抗氧化剂B组成的混合抗氧化剂。该方法可操作性良好，可以使用少量的抗氧化剂使聚合物充分终止，能够制造具有较不均匀的增塑剂吸收性并且具有良好的抗起始变色性和良好的热稳定性的氯乙烯聚合物。

8. 发明授权

US06355743B1 Process for producing vinyl chloride polymer in the presence of a chelating agent 失效
标题翻译：在螯合剂存在下生产氯乙烯聚合物的方法
公开(公告)号：US06355743B1
公开(公告)日：2002-03-12
申请号：US09410628
申请日：1999-10-01
申请人： Makoto Ooura , Kaname Inoue , Masakuni Yamamoto , Tadashi Amano
发明人： Makoto Ooura , Kaname Inoue , Masakuni Yamamoto , Tadashi Amano
IPC分类号： C08F220
CPC分类号： C08F2/004 , B01J19/18 , B01J2219/00081
摘要： In a process for producing vinyl chloride polymers including polymerization of vinyl chloride or a monomer mixture containing it in an aqueous medium using a polymerization initiator, the polymerization is carried out in the presence of a chelating agent. The chelating agent is capable of chelating iron (II) and iron (III). This process makes it possible to prevent polymer scales from adhering to, e.g. baffle surfaces facing inner walls of the polymerization vessel, which has been hitherto difficult to do so, and less cause initial discoloration of polymer products to improve quality. It is more effective to use a polymerization vessel previously provided with coating films of a polymer scale preventive agent on the inner walls of the polymerization vessel and the other portions with which monomers come into contact in the course of polymerization.
摘要翻译：在使用聚合引发剂的含水介质中使用氯乙烯聚合或含有它们的单体混合物的氯乙烯聚合物的制造方法中，在螯合剂的存在下进行聚合。螯合剂能够螯合铁（II）和铁（III）。该方法使得可以防止聚合物垢附着到例如面对迄今为止难以做到的聚合容器的内壁的挡板表面，并且较少导致聚合物产品的初始变色以改善质量。在聚合容器的内壁和聚合反应过程中单体接触的其它部分使用预先设有聚合物防垢剂的涂膜的聚合容器更为有效。

9. 发明授权

US6022932A Process for producing vinyl chloride polymer, with iron chelates in coated vessel 失效
标题翻译：生产氯乙烯聚合物的方法，在包衣容器中用铁螯合物
公开(公告)号：US6022932A
公开(公告)日：2000-02-08
申请号：US848196
申请日：1997-04-29
申请人： Makoto Ooura , Kaname Inoue , Masakuni Yamamoto , Tadashi Amano
发明人： Makoto Ooura , Kaname Inoue , Masakuni Yamamoto , Tadashi Amano
IPC分类号： B01J19/18 , C08F2/00 , C08F2/20
CPC分类号： C08F2/004 , B01J19/18 , B01J2219/00081
摘要： In a process for producing vinyl chloride polymers including polymerization of vinyl chloride or a monomer mixture containing it in an aqueous medium using a polymerization initiator, the polymerization is carried out in the presence of a chelating agent, The chelating agent is capable of chelating iron (II) and iron (III). This process makes it possible to prevent polymer scales from adhering to, e.g. baffle surfaces facing inner walls of the polymerization vessel, which has been hitherto difficult to do so, and less cause initial discoloration of polymer products to improve quality. It is more effective to use a polymerization vessel previously provided with coating films of a polymer scale preventive agent on the inner walls of the polymerization vessel and the other portions with which monomers come into contact in the course of polymerization.
摘要翻译：在使用聚合引发剂的含水介质中含氯乙烯聚合或含有它们的单体混合物的氯乙烯聚合物的制造方法中，聚合在螯合剂的存在下进行。螯合剂能够螯合铁（ II）和铁（III）。该方法使得可以防止聚合物垢附着到例如面对迄今为止难以做到的聚合容器的内壁的挡板表面，并且较少导致聚合物产品的初始变色以改善质量。在聚合容器的内壁和聚合反应过程中单体接触的其它部分使用预先设有聚合物防垢剂的涂膜的聚合容器更为有效。

10. 发明授权

US06600000B1 Process for producing vinyl chloride polymer by means of a uniaxial eccentric screw pump 失效
标题翻译：通过单轴偏心螺杆泵生产氯乙烯聚合物的方法
公开(公告)号：US06600000B1
公开(公告)日：2003-07-29
申请号：US09511317
申请日：2000-02-23
申请人： Makoto Ooura , Tadashi Amano
发明人： Makoto Ooura , Tadashi Amano
IPC分类号： C08F1406
CPC分类号： C08F14/06 , C08K5/13 , C08F2/44 , C08L27/06
摘要： A process for producing a vinyl chloride polymer, the process including the steps of charging into a polymerization vessel, vinyl chloride or a monomer mixture containing vinyl chloride, water, and other materials necessary for polymerization, and polymerizing in an aqueous medium the vinyl chloride or the monomer mixture. An antioxidant is added to a mixture of materials before polymerization, or to a polymerization reaction mixture during polymerization or after polymerization. The antioxidant is added in the state of an aqueous dispersion and by means of a uniaxial eccentric screw pump. The aqueous antioxidant dispersion can be added at a constant rate and stably, without causing any block-up of the interior of the pump even when the polymerization vessel is held at a high internal pressure. Hence, vinyl chloride polymers having less uneven plasticizer absorption and having good anti-initial discoloration properties and thermal stability can be produced stably.
摘要翻译：一种制备氯乙烯聚合物的方法，该方法包括以下步骤：将聚合容器，氯乙烯或含有氯乙烯，水和聚合所需的其它物质的单体混合物装入聚合容器中，并在水性介质中聚合氯乙烯或单体混合物。在聚合前将抗氧化剂加入到材料的混合物中，或在聚合期间或聚合后加入到聚合反应混合物中。抗氧化剂以水分散体的状态并通过单轴偏心螺杆泵加入。即使在将聚合容器保持在高内压下时，可以以恒定的速率和稳定地加入水性抗氧化剂分散体，而不引起泵的内部的任何堵塞。因此，可以稳定地制造具有不均匀的增塑剂吸收性和良好的抗起始变色性和热稳定性的氯乙烯聚合物。

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