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    • 1. 发明专利
    • Spinning stock solution of polyacrylonitrile-based fibers, and method for producing the same
    • 基于聚丙烯酰基纤维素的纺丝纺丝溶液及其制备方法
    • JP2010059560A
    • 2010-03-18
    • JP2008224680
    • 2008-09-02
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • FUKUBA YOSHINORIFUTAI TAKESHI
    • D01F6/54C08L33/20
    • PROBLEM TO BE SOLVED: To provide a spinning stock solution of polyacrylonitrile-based fibers which is excellent in balance of shearing viscosity and spinnability, and makes a PAN (polyacrylonitrile)-based polymer in the spinning stock solution have a maximum concentration as much as possible, and to provide a method for producing the spinning stock solution of the polyacrylonitrile-based fibers.
      SOLUTION: The spinning stock solution of the polyacrylonitrile-based fibers is provided which contains 13-25 mass% polyacrylonitrile-based polymer having a mass-average molecular weight of 300,000-1,000,000, and containing 0.002-0.2 mass% of a polymer having a molecular weight of 3,000,000 or more, and 0.005-0.1 mass% of a polymer having a molecular weight of 20,000 or less. Further, the method for producing the spinning stock solution of the polyacrylonitrile-based fibers is provided.
      COPYRIGHT: (C)2010,JPO&INPIT
    • 要解决的问题:为了提供剪切粘度和可纺性的平衡优异的聚丙烯腈系纤维的纺丝原液,使纺丝原液中的PAN(聚丙烯腈)系聚合物的最大浓度为 并且提供一种聚丙烯腈系纤维的纺丝原液的制造方法。 解决方案:提供聚丙烯腈系纤维的纺丝原液,其含有质量平均分子量为30万〜100万的13-25质量%的聚丙烯腈系聚合物,含有0.002〜0.2质量%的聚合物 分子量为3,000,000以上,0.005〜0.1质量%的分子量为20,000以下的聚合物。 此外,提供了聚丙烯腈系纤维的纺丝原液的制造方法。 版权所有(C)2010,JPO&INPIT
    • 2. 发明专利
    • Method for producing acrylonitrile-based polymer
    • 生产基于丙烯腈的聚合物的方法
    • JP2010006967A
    • 2010-01-14
    • JP2008168570
    • 2008-06-27
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • SHIBATANI HARUMIFUTAI TAKESHISHIMOZAWA NOBUYUKIAOYAMA NAOKI
    • C08F6/24C08F2/18C08F20/44
    • PROBLEM TO BE SOLVED: To produce an acrylonitrile-based polymer, which allows good passability during a filtration process when using it as a spinning stock solution, by an aqueous deposition continuous polymerization procedure.
      SOLUTION: In a polymerization process, until a polymerization elapsed time from a polymerization starting time reaches at least 10 times of an average residence time, a volume-average particle diameter P of polymer particles in a polymer suspension liquid obtained at a polymerization elapsed time T is regularly measured, and a maximum value P
      max among the measure volume-average particle diameters P is found. A polymerization elapsed time Tn, at which a volume-average particle diameter P
      n equal to or larger than 85% of the maximum value P
      max is measured for the first time, is found. The polymer suspension liquid obtained after the polymerization elapsed time Tn is fractionated, and on this polymer suspension liquid, the following moisture removal process is performed.
      COPYRIGHT: (C)2010,JPO&INPIT
    • 要解决的问题:为了制备丙烯腈类聚合物,当通过水性沉积连续聚合方法将其用作纺丝原液时,在过滤过程中允许良好的通过性。 解决方案:在聚合过程中,直到聚合开始时间的聚合时间达到平均停留时间的至少10倍,聚合物颗粒在聚合物悬浮液中的体积平均粒径P在聚合反应中获得 经过时间T被测量,并且测量体积平均粒径P中的最大值P max 。 第一次测量等于或大于最大值P max 的85%的体积平均粒径P n 的聚合时间Tn, 被发现。 在聚合时间Tn后得到的聚合物悬浊液分馏,在该聚合物悬浊液上进行以下除湿处理。 版权所有(C)2010,JPO&INPIT
    • 3. 发明专利
    • Method for producing acrylonitrile-based precursor fiber
    • 生产基于丙烯腈的前置纤维的方法
    • JP2009287146A
    • 2009-12-10
    • JP2008142445
    • 2008-05-30
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • MATSUMURA HIROKOFUJII YASUYUKIFUTAI TAKESHI
    • D01F6/18D01D4/02D01F9/22
    • PROBLEM TO BE SOLVED: To provide a method by which an atmosphere of a gas layer between a discharge surface of a spinneret and a liquid surface of a coagulation bath is kept uniform without using a device for spinning of a complicated structure when spinning is carried out by a dry-jet wet spinning method and acrylonitrile-based precursor fibers having a dense surface and high homogeneity can be produced even when a spinning environment fluctuates.
      SOLUTION: The method for producing the acrylonitrile-based precursor fibers includes a dope preparing step of dissolving an acrylonitrile-based polymer containing 90 mass% or more of acrylonitrile in a solvent, regulating the polymer concentration to 17-25 mass%, and keeping the spinning dope at 50-80°C, and a spinning step of discharging the spinning dope from the spinneret having 50 to 500 discharge holes having a hole diameter of 0.02-0.5 mm and disposed at a pitch between the holes of 0.5 to 3.5 mm at 0.2-20 g/h based on one discharge hole, running the dope through the gas layer having a distance from the discharge surface of the spinneret to the liquid surface of the coagulation bath of 2-25 mm, and then directly introducing the dope into the coagulation bath at a temperature of 0-30°C, and having a concentration of an organic solvent of 70-90 mass%.
      COPYRIGHT: (C)2010,JPO&INPIT
    • 要解决的问题:提供一种方法,其中喷丝板的喷出表面和凝固浴的液面之间的气体层的气氛保持均匀,而不需要在旋转时使用复杂结构的纺丝装置 通过干式喷射湿式纺丝法进行,即使纺丝环境波动,也可以制造具有致密表面,高均匀性的丙烯腈系前体纤维。 解决方案:制备丙烯腈基前体纤维的方法包括将溶剂中含有90质量%以上丙烯腈的丙烯腈系聚合物溶解在溶剂中的调色剂准备工序,将聚合物浓度调节为17〜25质量% 并将纺丝原液保持在50-80℃,以及纺丝步骤,将具有50至500个孔径的喷丝头的纺丝原液排出至孔径为0.02-0.5mm的排出孔,并以0.5至0.5的间距设置至 基于一个排出孔以0.2-20g / h的速度为3.5mm,通过从喷丝板的排出表面到凝固浴的液面的距离为2〜25mm的气体层,将涂料直接导入 在0-30℃的温度下将其掺入凝固浴中,并且有机溶剂的浓度为70-90质量%。 版权所有(C)2010,JPO&INPIT
    • 5. 发明专利
    • Production method of acrylonitrile-based polymer
    • 基于丙烯腈的聚合物的生产方法
    • JP2014162842A
    • 2014-09-08
    • JP2013034546
    • 2013-02-25
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • MATSUDA HARUMIAOYAMA NAOKIMATSUYAMA NAOMASAFUTAI TAKESHIHIROTA NORIFUMI
    • C08F6/00C08F20/44
    • PROBLEM TO BE SOLVED: To provide a production method of an acrylonitrile-based polymer that disintegrates only polymer agglomerates among large particles in a polymerization reaction liquid of an acrylonitrile-based polymer before filtration to efficiently remove only components having a harmful effect on solubility, and to provide the acrylonitrile-based polymer.SOLUTION: A production method of an acrylonitrile-based polymer includes a step for polymerizing a monomer containing 90 mass% or more of an acrylonitrile unit in water or a solvent in a polymerization reactor using a redox catalyst as a polymerization initiator, a step for adding a polymerization terminator to the polymerization reaction liquid discharged from the polymerization reactor, a step for disintegrating agglomerates of polymer particles contained in the polymerization reaction liquid added with the polymerization terminator, and a step for filtering the polymerization reaction liquid.
    • 要解决的问题:提供一种丙烯腈系聚合物的制造方法,其在过滤之前仅在丙烯腈系聚合物的聚合反应液中的大颗粒之间仅分解聚合物附聚物,仅有效除去对溶解度有害的成分, 丙烯腈系聚合物的制造方法包括使用氧化还原催化剂将含有90质量%以上丙烯腈单元在水或溶剂中的单体聚合的聚合反应器的步骤 聚合引发剂,向从聚合反应器排出的聚合反应液中添加聚合终止剂的步骤,将聚合反应液中添加的聚合反应液中所含的聚合物粒子的聚集体粒子粉碎的工序和聚合反应过程 液体。
    • 6. 发明专利
    • Acrylonitrile-based copolymer for carbon fiber
    • 用于碳纤维的基于丙烯腈的共聚物
    • JP2012214657A
    • 2012-11-08
    • JP2011081826
    • 2011-04-01
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • UNOKI SAEFUTAI TAKESHIHIROTA NORIFUMIAOYAMA NAOKINIIMEN YUSUKE
    • C08F220/44D01F6/18
    • PROBLEM TO BE SOLVED: To provide an acrylonitrile-based copolymer in which the solubility in a solvent is improved to enhance the stability in the production process of a polyacrylonitrile-based fiber by reducing a load on a filter in a filtration process during fiber spinning.SOLUTION: When fractionating a component every 5 mass% based on the peak area derived from the acrylonitrile-based copolymer in a GPC measurement, the copolymer satisfies the relation, 1.30>(A)/(B)>0.80 [wherein (A) is a mass ratio of components except an acrylonitrile unit in each fractionation therafter; and (B) is a mass ratio of components except the acrylonitrile unit in the copolymer before fractionation].
    • 要解决的问题:提供一种丙烯腈系共聚物,其中溶剂中的溶解度得到改善,以通过在过滤过程中减小过滤器上的负荷来提高聚丙烯腈基纤维的生产过程中的稳定性 纤维纺丝。 < P>解决方案:在GPC测定中,基于丙烯腈系共聚物衍生的峰面积,每5质量%分数成分,共聚物满足关系式1.30>(A)/(B)> 0.80 [ A)是每个分馏器中除丙烯腈单元之外的组分的质量比; 和(B)是分馏前共聚物中丙烯腈单元除外的成分的质量比]。 版权所有(C)2013,JPO&INPIT
    • 8. 发明专利
    • Method for producing acrylonitrile-based fiber as carbon fiber precursor
    • 用于生产基于丙烯腈的纤维作为碳纤维前体的方法
    • JP2008303500A
    • 2008-12-18
    • JP2007151794
    • 2007-06-07
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • FUTAI TAKESHI
    • D01F6/18D01F6/54D01F9/22
    • PROBLEM TO BE SOLVED: To provide a suitable method for producing a high-performance acrylonitrile-based fiber as a carbon fiber precursor, in high productivity and in high degree of freedom of its composition design.
      SOLUTION: The method for producing the acrylonitrile-based fiber as a carbon fiber precursor comprises blending (A) a carboxyl-free acrylonitrile-based polymer with (B) a carboxyl-containing acrylonitrile-based polymer followed by spinning the blend. In this method, it is preferable that the polymer B contain 0.014-100 mass% of carboxyl-containing monomer units and the mass ratio B/A be 0.0001-2.3.
      COPYRIGHT: (C)2009,JPO&INPIT
    • 要解决的问题:提供一种用于以高生产率和高自由度地制备作为碳纤维前体的高性能丙烯腈基纤维的合适方法。 解决方案:制备作为碳纤维前体的丙烯腈系纤维的方法包括将(A)无羧基丙烯腈系聚合物与(B)含羧基的丙烯腈系聚合物混合,然后纺丝共混物。 在该方法中,优选聚合物B含有0.014〜100质量%的含羧基的单体单元,质量比B / A为0.0001〜2.3。 版权所有(C)2009,JPO&INPIT
    • 10. 发明专利
    • Method for controlling quality of carbon fiber precursor acrylic fiber
    • 控制碳纤维前纤丙烯纤维质量的方法
    • JP2012211814A
    • 2012-11-01
    • JP2011077414
    • 2011-03-31
    • Mitsubishi Rayon Co Ltd三菱レイヨン株式会社
    • FUTAI TAKESHIMATSUYAMA NAOMASAHIROTA NORIFUMI
    • G01N25/20D01F6/18D01F9/22
    • PROBLEM TO BE SOLVED: To provide a method for distinguishing carbon fiber precursor fiber containing such an amount of iron elements as to decrease strength more simply.SOLUTION: A method for controlling quality of carbon fiber precursor acrylic fiber comprises the following four steps: (1) baking carbon fiber precursor acrylic fiber containing less than 0.5 ppm of iron and carbon fiber precursor acrylic fiber containing 0.5 ppm of iron or greater under the same baking conditions to obtain carbon fibers; (2) calculating strand strength of each carbon fiber obtained in the step 1 above and calculating percentage content of iron that causes strength decrease ratio to fall into a range from 0.5% to 20%, the strength decrease ratio being the ratio of strand strength of carbon fiber obtained by baking the carbon fiber precursor acrylic fiber containing less than 0.5 ppm of iron to that of carbon fiber obtained by baking the carbon fiber precursor acrylic fiber containing 0.5 ppm of iron or greater; (3) measuring, under the same conditions, calorific value at the shoulder of a calorific peak around three minutes after the start of measurement by DSC in the atmosphere at constant temperatures 190 to 270°C for the carbon fiber precursor acrylic fiber containing less than 0.5 ppm of iron and the carbon fiber precursor acrylic fiber containing iron that decreases the strength 0.5 to 20%; and (4) detecting process failure based on the difference of calorific peak obtained in the step 3.
    • 要解决的问题:提供一种区分含有这种量的铁元素的碳纤维前体纤维以更简单地降低强度的方法。 解决方案:一种控制碳纤维前体丙烯酸纤维质量的方法包括以下四个步骤:(1)烘烤含有0.5ppm铁的铁和碳纤维前体丙烯酸纤维含量小于0.5ppm的碳纤维前体丙烯酸纤维,或 在相同的烘烤条件下更大以获得碳纤维; (2)计算上述步骤1中获得的每种碳纤维的线强度,并计算使强度降低率落入0.5%至20%的范围内的铁含量,强度降低率为线强度比 通过将含有小于0.5ppm铁的碳纤维前体丙烯酸纤维烘烤通过焙烧含有0.5ppm或更大的铁的碳纤维前体丙烯酸纤维而获得的碳纤维获得的碳纤维; (3)在相同的条件下,测量开始测量三分钟后发热峰值的热值在大气中在190〜270℃的恒温下测定,含碳纤维前体丙烯酸纤维含量小于 0.5ppm的铁和含有铁的碳纤维前体丙烯酸纤维,其强度降低0.5〜20%; (4)基于步骤3中获得的发热峰的差异来检测过程故障。(C)2013,JPO和INPIT