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公开(公告)号：US5282680A
公开(公告)日：1994-02-01
申请号：US63604
申请日：1993-05-19
CPC分类号： B01F5/16 , B01J19/2415 , B01J19/243 , B01J2219/00094 , B01J2219/00162 , B01J2219/00164 , B01J2219/00182
摘要： An apparatus for continuous polymerization of vinyl chloride or a vinyl chloride-based monomeric mixture, comprising a pre-mixer 1 for preparing an aqueous suspension of the vinyl chloride or vinyl chloride-based monomeric mixture, and a polymer slurry tank 5 connected to the pre-mixer 1 through a polymerization passage comprising a piping 3, wherein a pump comprising a conical hub and an impeller mounted thereon comprised of a single spiral blade is used for drawing out the aqueous suspension from the pre-mixer into the polymerization passage and for discharging a polymer slurry formed in the passage into the slurry tank, and the polymerization passage has a length sufficient for permitting the vinyl chloride or vinyl chloride-based monomeric mixture contained in the aqueous suspension flowing through the passage to be polymerized to a predetermined extent while passing through the passage. The use of the pump having the structure as above ensures a marked suppression of polymer scale deposition in the pump, heat exchanger and pipings, and makes it possible to produce a resin with few fish-eyes. The apparatus is of extremely high industrial value for carrying out continuous polymerization.
摘要翻译： 一种用于氯乙烯或氯乙烯基单体混合物的连续聚合的装置，包括用于制备氯乙烯或氯乙烯基单体混合物的水悬浮液的预混合器1和连接到前述聚合物浆料罐5的聚合物浆料罐5。 混合器1通过包括管道3的聚合通道，其中包括圆锥形轮毂和安装在其上的叶轮由包括单个螺旋叶片的泵用于将预混合器中的水悬浮液抽出到聚合通道中并用于排出 聚合物淤浆形成在通入浆料罐的通道中，并且聚合通道的长度足以允许流过通道的含水悬浮液中所含的氯乙烯或氯乙烯类单体混合物在通过时聚合至预定程度 通过通道。 具有上述结构的泵的使用确保了泵，热交换器和管道中的聚合物垢沉积的显着抑制，并且使得可以生产几乎没有鱼眼的树脂。 该设备具有非常高的工业价值用于进行连续聚合。
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2.发明授权Polymerization of vinyl chloride with hydroxycarboxylic acids, inhibitors and Fe ions 失效用羟基羧酸，抑制剂和Fe离子聚合氯乙烯公开(公告)号：US06455646B1
公开(公告)日：2002-09-24
申请号：US09988524
申请日：2001-11-20
申请人： Masahiro Usuki , Minoru Shigemitsu , Tadashi Amano
发明人： Masahiro Usuki , Minoru Shigemitsu , Tadashi Amano
IPC分类号： C08F216
摘要： Vinyl chloride or a monomer mixture containing it transported over a long distance or stored for a long period usually contains a polymerization inhibitor and Fe ions. If this kind of vinyl chloride or monomer mixture is polymerized, stirring torque during the polymerization increases, and heat removal by the cooling jacket of a polymerization vessel tends to become insufficient, making the polymer quality subject to bad influences. In the present invention, a hydroxycarboxylic acid compound is added to the polymerization mixture in an amount of 50-1000 ppm relative to the monomer or monomer mixture. As a result, an increase in stirring torque during polymerization is suppressed, and heat removal by the cooling jacket of the polymerization vessel can be performed effectively, making it possible to obtain vinyl chloride of good quality.
摘要翻译： 氯乙烯或含有长距离运输或长期储存的单体混合物通常含有阻聚剂和Fe离子。 如果这种氯乙烯或单体混合物聚合，聚合过程中的搅拌转矩增加，聚合容器的冷却套的散热倾向变得不足，使聚合物质量受到不良影响。 在本发明中，羟基羧酸化合物相对于单体或单体混合物以50-1000ppm的量加入到聚合混合物中。 结果，抑制了聚合过程中搅拌转矩的增加，并且能够有效地进行聚合容器的冷却套的散热，能够得到质量好的氯乙烯。
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3.发明申请DISPERSION STABILIZER FOR SUSPENSION POLYMERIZATION AND METHOD OF PRODUCING VINYL CHLORIDE-BASED POLYMER USING SAME 审中-公开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
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。
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4.发明授权Process for producing vinyl chlorine-based polymer via continuous or intermittent addition of dispersing stabilizer 失效通过连续或间歇加入分散稳定剂生产氯乙烯基聚合物的方法
公开(公告)号：US5376747A
公开(公告)日：1994-12-27
申请号：US125764
申请日：1993-09-24
申请人： Minoru Shigemitsu , Tadashi Amano
发明人： Minoru Shigemitsu , Tadashi Amano
CPC分类号： C08F14/06
摘要： A process for suspension polymerizing vinyl chloride or a monomeric mixture containing the same in an aqueous medium comprising the step of adding a partially saponified polyvinyl alcohol having an average polymerization degree of 600 to 800 and a saponification degree of 65 to 75 mol % to a polymerization system, wherein the partially saponified polyvinyl alcohol is added before start of polymerization, and also after-added continuously or intermittently over the period from the start of polymerization to the time when a polymerization conversion of 10 to 30% is reached. By the suspension polymerization process, it is possible to obtain a vinyl chloride-based polymer having high bulk specific gravity, high gelation rate and a certain level of thermal stability and showing an effectively reduced number of fish eyes when formed into shaped products.
摘要翻译： 一种在水性介质中悬浮聚合氯乙烯或含有该氯乙烯的单体混合物的方法，包括将平均聚合度为600〜800，皂化度为65〜75摩尔％的部分皂化聚乙烯醇加入到聚合 系统，其中在聚合开始之前加入部分皂化的聚乙烯醇，并且在从聚合开始到达到10至30％的聚合转化的时间期间连续或间歇地后加入。 通过悬浮聚合方法，可以得到体积比重高，凝胶化率高，热稳定性一定的氯乙烯类聚合物，形成成型品时可以有效减少鱼眼数量。
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5.发明授权Method for recovering unreacted monomers after preparation of vinylic polymer 失效制备乙烯基聚合物后回收未反应单体的方法
公开(公告)号：US5212265A
公开(公告)日：1993-05-18
申请号：US859814
申请日：1992-03-30
申请人： Tadashi Amano , Minoru Shigemitsu
发明人： Tadashi Amano , Minoru Shigemitsu
CPC分类号： C08F6/003
摘要： A method for recovering unreacted monomers during preparation of a vinylic polymer comprises the steps of polymerizing a vinyl monomer in an aqueous medium in a polymerizer and then recovering unreacted monomers from the polymerization system, wherein a gas evacuation rate per unit charge weight of the monomer is controlled to the range of from 60 to 300 Nm.sup.3 /hr per ton of the monomer from the initiation of the monomer recovery till the pressure in the polymerizer reaches 2.5 kg/cm.sup.2 G and a superficial gas linear velocity is reduced to a level of not more than 0.008 m/sec when the pressure in the polymerizer reaches 2.5 kg/cm.sup.2 G. The method makes it possible to recover unreacted monomers quickly without causing carrying over of polymer particles formed and is effective to maintain high quality of vinylic polymers produced.
摘要翻译： 在制备乙烯基聚合物期间回收未反应单体的方法包括以下步骤：在聚合反应器中的水性介质中聚合乙烯基单体，然后从聚合体系中回收未反应的单体，其中单体单位电荷重量的排气速率为 控制在从单体回收开始直到聚合器中的压力达到2.5kg / cm2G的每吨单体为60至300Nm 3 / hr的范围内，并且表观气体线速度降低到不超过 当聚合器中的压力达到2.5kg / cm2G时为0.008m / sec。 该方法使得可以快速回收未反应的单体而不会导致形成的聚合物颗粒的携带，并且有效地保持所生产的乙烯基聚合物的高质量。
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公开(公告)号：US5357011A
公开(公告)日：1994-10-18
申请号：US159248
申请日：1993-11-30
申请人： Shuji Ohnishi , Tadashi Amano
发明人： Shuji Ohnishi , Tadashi Amano
CPC分类号： C08F14/06
摘要： A process for producing a vinyl chloride-based polymer, which comprises suspension polymerizing vinyl chloride monomer or a vinyl chloride-containing monomeric mixture in an aqueous medium in the presence of an oil-soluble polymerization initiator, wherein the initiator comprises (A) at least one compound having a 10-hour half-life temperature, at a concentration of 0.1 mol/l in benzene, of not lower than 35.degree. C., and (B) at least one compound having a 10-hour half-life temperature, at a concentration of 0.1 mol/l in benzene, of lower than 35.degree. C., with the amount of the initiator (B) being from 0.01 to 0.07% by weight based on the monomer or monomeric mixture and being from 10 to 30% by weight based on the total amount of the initiators (A) and (B). The process makes it possible to shorten easily the time required for raising temperature, and to produce vinyl chloride-based polymers which have a good particle size distribution and which have few fish eyes when formed into sheets or the like.
摘要翻译： 一种氯乙烯类聚合物的制造方法，其特征在于，在油溶性聚合引发剂的存在下，在含水介质中使氯乙烯单体或含氯乙烯单体混合物悬浮聚合，其中，所述引发剂至少包含（A） 一种化合物，其在苯中的浓度为0.1mol / l的半衰期为10小时，不低于35℃，和（B）至少一种具有10小时半衰期的化合物， 在苯中浓度为0.1mol / l，低于35℃，引发剂（B）的量基于单体或单体混合物为0.01至0.07重量％，为10至30重量％ （A）和（B）的总量。 该方法可以容易地缩短提高温度所需的时间，并且可以制备具有良好粒度分布且在形成片状等时几乎没有鱼眼的氯乙烯基聚合物。
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公开(公告)号：US5348708A
公开(公告)日：1994-09-20
申请号：US989569
申请日：1992-12-11
申请人： Tadashi Amano , Shuji Ohnishi
发明人： Tadashi Amano , Shuji Ohnishi
CPC分类号： B01J19/1881 , B01J19/002 , B01J19/1806 , C08F2/00 , B01J2219/00252
摘要： A polymerizing apparatus for polymerizing a monomer having an ethylenically unsaturated double bond which is equipped with a polymerization vessel having an agitator and a return nozzle to a gaseous phase part and with a circulating pipeline extending from said polymerization vessel and connected to said return nozzle of the polymerization vessel through a heat exchanger, in which said return nozzle is installed such that it discharges a reaction mixture in the direction which is tangential to the circumferential wall of the vessel and in which the agitator is rotated. Scale of a polymer can be prevented from depositing in the polymerization vessel and it is possible to reduce the number of fish eyes of a molded product such as a sheet into which the polymer obtained by the present polymerizing apparatus can be worked.
摘要翻译： 一种聚合装置，用于使具有烯键式不饱和双键的单体聚合，该单体装备有具有搅拌器和返回喷嘴的聚合容器至气相部分，并具有从所述聚合容器延伸并连接到所述聚合反应器的所述返回喷嘴的循环管线 聚合容器通过热交换器安装，其中所述返回喷嘴安装成使得其沿与容器的圆周壁相切的方向排出反应混合物，并且搅拌器旋转。 可以防止聚合物的鳞片沉积在聚合容器中，并且可以减少通过本聚合装置获得的聚合物可以加工的成型产品例如片材的鱼眼数量。
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8.发明授权
公开(公告)号：US5612437A
公开(公告)日：1997-03-18
申请号：US364449
申请日：1994-12-27
申请人： Takuya Ueda , Kikuo Nakajima , Yoichi Tanifuji , Tadashi Amano , Shuji Ohnishi
发明人： Takuya Ueda , Kikuo Nakajima , Yoichi Tanifuji , Tadashi Amano , Shuji Ohnishi
CPC分类号： B01J19/18 , B01J19/0013 , C08F14/06 , B01J2219/00081 , B01J2219/185 , B01J2219/1943
摘要： A vinyl chloride polymer is produced by subjecting vinyl chloride or a monomer mixture made up mainly of vinyl chloride to suspension polymerization in an aqueous medium using a polymerization apparatus equipped with a polymerization vessel. The polymerization apparatus used comprises a polymerization vessel (1) having a substantially cylindrical inner space, said inner space of said polymerization vessel being provided with a plurality of baffles (5) comprising vertically extending pipes, and serpentine pipelines (6) each of which is placed between two adjacent baffles and is extended in a serpentine fashion along the polymerization vessel inner wall from the lower part to the upper part of the polymerization vessel, and a refrigerant being passed through said baffles and said serpentine pipelines. High-cooling performance can be obtained, a high-speed reaction in a large-sized polymerization vessel becomes possible, and a stable polymerization reaction can be carried out. A high-quality and uniform polymer that has few fish eyes and has a high bulk specific gravity can be obtained.
摘要翻译： 使用装有聚合容器的聚合装置，将氯乙烯或主要由氯乙烯组成的单体混合物在含水介质中进行悬浮聚合来制备氯乙烯聚合物。 使用的聚合装置包括具有基本上圆柱形的内部空间的聚合容器（1），所述聚合容器的内部空间设置有多个包括垂直延伸的管道的挡板（5）和蛇形管道（6） 放置在两个相邻的挡板之间，并且沿着聚合容器内壁从聚合容器的下部延伸到上部延伸，并且制冷剂通过所述挡板和所述蛇形管道。 可以获得高冷却性能，可以在大型聚合容器中进行高速反应，并且可以进行稳定的聚合反应。 可以获得鱼眼少且体积比重高的高质量且均匀的聚合物。
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公开(公告)号：US5449723A
公开(公告)日：1995-09-12
申请号：US126378
申请日：1993-09-24
申请人： Tadashi Amano , Shuji Ohnishi
发明人： Tadashi Amano , Shuji Ohnishi
CPC分类号： C08F2/002 , B01J19/002 , B01J19/1881 , B01J19/2435 , B01J19/2465 , B01J2219/00094 , B01J2219/00103 , B01J2219/00114 , B01J2219/00252
摘要： An improvement is proposed in the method for the preparation of a polyvinyl chloride resin by the suspension polymerization of the monomer in a polymerization reactor system comprising a reactor and an external heat exchanger connected to the reactor by a pipe line through a pumping means in order to supplement the deficiency in the cooling capacity of the jacket of the reactor and/or reflux condenser installed thereto when the capacity of the reactor is greatly increased. While such an external circulating circuit using a conventional pump suffers from a serious problem of polymer scale deposition on the inner walls of the circuit and downgrading of the quality of the resin product, these drawbacks can be dissolved by using a specific pump having an impellor in the form of a single spiral screw blade around a hub having a conical configuration to circulate the polymerization mixture through the heat exchanger for the removal of the heat of polymerization, which is started at or after the moment when the temperature of the polymerization mixture in the reactor reaches the predetermined polymerization temperature but before the conversion of the monomer to polymer exceeds 10%.
摘要翻译： 通过单体在包括反应器和外部热交换器的聚合反应器系统中的悬浮聚合的方法中提出了改进方案，该反应器和外部热交换器通过泵送装置通过管线连接到反应器，以便 补充了当反应器的容量大大增加时，安装在其上的反应器和/或回流冷凝器的夹套的冷却能力的不足。 虽然使用常规泵的这种外部循环回路存在聚合物垢沉积在电路内壁上并严重降低树脂产品质量的严重问题，但这些缺点可以通过使用具有叶轮的特定泵来溶解 围绕具有圆锥形构造的单螺旋螺旋叶片的形式，以使聚合混合物循环通过热交换器以消除聚合热，该聚合混合物在聚合混合物的温度 反应器达到预定的聚合温度，但在单体转化为聚合物之前超过10％。
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公开(公告)号：US5328666A
公开(公告)日：1994-07-12
申请号：US4567
申请日：1993-01-14
申请人： Tadashi Amano , Shuji Ohnishi
发明人： Tadashi Amano , Shuji Ohnishi
CPC分类号： B01J19/2465 , B01J19/002 , B01J19/24 , B01J19/2435
摘要： In a polymerizing apparatus which comprises a polymerization vessel and a circulating line comprising a heat exchanger installed outside said polymerization vessel and a circulating pipeline extending from said polymerization vessel and returning to said polymerization vessel through said heat exchanger, the improvement comprising a strainer installed in the course of said circulating pipeline. Since polymer scale and a polymer in the form of blocks formed in the circulating line can be trapped, the circulating pipeline and tubes of the heat exchanger can be prevented from being blocked up. Further, since they can be prevented from mixing with a reaction mixture in the polymerization vessel, when the obtained polymer is worked into a molded item such as a sheet, fish eyes can be prevented from increasing. Therefore, a polymer can be produced efficiently with high productivity.
摘要翻译： 在包括聚合容器和包括安装在所述聚合容器外部的热交换器的循环管线的循环管线和从所述聚合容器延伸并通过所述热交换器返回到所述聚合容器的循环管道的聚合装置中，改进包括安装在所述聚合容器中的过滤器 循环管道过程。 由于聚合物垢和在循环管线中形成的块状聚合物可以被捕获，所以可以防止热交换器的循环管道和管堵塞。 此外，由于可以防止它们与聚合容器中的反应混合物混合，所以当将所得的聚合物加工成片状的成型品时，可以防止鱼眼的增加。 因此，可以高效率地生产聚合物。
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