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    • 1. 发明专利
    • Recovery of trioxane
    • 三氧化二铁的恢复
    • JPS59196886A
    • 1984-11-08
    • JP7144183
    • 1983-04-25
    • Asahi Chem Ind Co Ltd
    • SEKIYA HARUTAKAMASAMOTO JIYUNZOUMATSUZAKI KAZUHIKO
    • C07D323/06
    • PURPOSE: To recover trioxane containing no triethylamine effectively in high purity, by adding an acid to an aqueous phase containing trioxane and triethylamine after synthesis of copolymer of trioxane and ethylene oxide is over.
      CONSTITUTION: Trioxane is copolymerized with ethylene oxide in the presence of a boron trifluoride compound, the copolymer is brought into contact with a triethylamine (TEA for short)-containing aqueous solution, the solution is filtered, an aqueous solution containing trioxane and TEA is fed to the distillation column I , a trioxane-containing aqueous solution is fed from the bottom of the column to the distillation column II, an nonaqueous organic solvent (e.g., benzene) is fed from 5 to a distillation containing trioxane and water from the heat of the column, trioxane is transferred to an organic phase, taken out from 6, the aqueous phase is circulated from 7 to the distillation column II to recover trioxane. In the operation, an acid (e.g., formic acid) is fed from any of the feed openings 9W13 so trioxane containing no TEA is recovered.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:通过在三恶烷和环氧乙烷的共聚物合成后,通过向含有三恶烷和三乙胺的水相中加入酸来回收高纯度不含三乙胺的三恶烷。 构成:三氟化硼在三氟化硼化合物的存在下与环氧乙烷共聚,共聚物与三乙胺(简称TEA)的水溶液接触,过滤溶液,加入含有三恶烷和TEA的水溶液 向蒸馏塔I中,将含三恶烷的水溶液从塔底部进料到蒸馏塔II中,将非水有机溶剂(例如苯)从5加入到含有三恶烷和水的蒸馏中, 将柱,三恶烷转移到有机相,从6中取出,水相从7循环到蒸馏塔II以回收三恶烷。 在操作中,酸(例如甲酸)从任何进料口9-13进料,因此回收不含TEA的三恶烷。
    • 2. 发明专利
    • Production of trioxane
    • 三氧化二铁的生产
    • JPS59134789A
    • 1984-08-02
    • JP671783
    • 1983-01-20
    • Asahi Chem Ind Co Ltd
    • MATSUZAKI KAZUHIKOMASAMOTO JIYUNZOU
    • C07D323/06B01J31/10C07B61/00
    • Y02P20/52
    • PURPOSE: To produce trioxane useful as a starting material of polyoxymethylene, in high efficiency, by contacting formaldehyde with a macronetwork cation exchange resin having sulfonic acid group.
      CONSTITUTION: The objective trioxane can be produced by contacting (A) formaldehyde containing preferably 0.05W14.0wt% of formic acid in a liquid phase (preferably a formaldehyde concentration of 30W75wt%) or a vapor phase (preferably a formaldehyde concentration of ≥75wt%) with (B) a macronetwork cation exchange resin having sulfonic acid group and having an ion exchange capacity of 0.85W2.55 mg-equivalent per 1ml of the swollen resin, preferably at 50W125°C in liquid phase, or 85W150°C in vapor phase for 2secW15min.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:通过使甲醛与具有磺酸基的大网络阳离子交换树脂接触,可以高效率地生产作为聚甲醛起始原料的三恶烷。 构成:目标三恶烷可以通过使(A)在液相(优选甲醛浓度为30-75重量%)中优选含有0.05-14.0重量%甲酸的甲醛或气相(优选甲醛浓度> = 75wt%)与(B)具有磺酸基并且每1ml溶胀树脂的离子交换容量为0.85-2.55mg当量的大分子阳离子交换树脂,优选在液相中为50-125℃,或 85-150℃气相2秒-15分钟。
    • 3. 发明专利
    • Production of trioxane
    • 三氧化二铁的生产
    • JPS58198482A
    • 1983-11-18
    • JP7958082
    • 1982-05-12
    • Asahi Chem Ind Co Ltd
    • HAMANAKA KATSUHIKOIWASAKO TOSHIYUKIMASAMOTO JIYUNZOU
    • C07D323/06
    • PURPOSE: In the production of trioxane by condensation of formaldehyde, the formaldehyde is fed in the form of a gas substantially free from water and further, the aqueous phase remaining after recovery of trioxane by extraction is refluxed to the reaction zone, thus giving trioxane advantageously.
      CONSTITUTION: Gaseous formaldehyde substantially free from water is fed as a raw material 1 to the reaction zone 2 where aqueous formaldehyde is evaporated in the presence of an acidic catalyst by heating and the evaporated vapor is introduced into the distillation zone 3. Then, the distillate from the distillation zone, containing trioxane is brought into contact with an organic solvent 4 which is a zeotropic with water and insoluble in water, preferably an aromtic hydrocarbon, especially benzene. Then, the resultant mixture is separated into the organic solvent phase containing trioxane and the aqueous phase 6 and trioxane is recovered from the former phase, while the latter phase is made to reflux to the reaction zone 2. Thus, trioxane used as a raw material for polyoxymethylene is obtained in high purity and high yield through a simplified process.
      COPYRIGHT: (C)1983,JPO&Japio
    • 目的:在通过甲醛缩合生产三恶烷时,甲醛以基本上不含水的气体的形式进料,此外,通过萃取回收三恶烷后残留的水相回流至反应区,有利于得到三恶烷 。 构成:将基本上不含水的气态甲醛作为原料1加入到反应区2中,在反应区2中,通过加热在酸性催化剂存在下蒸发甲醛水溶液,将蒸发的蒸气引入蒸馏区3.然后,蒸馏出的馏出物 从含有三恶烷的蒸馏区与有机溶剂4接触,有机溶剂4与水不共沸,不溶于水,优选芳烃,特别是苯。 然后,将所得混合物分离成含有三恶烷的有机溶剂相,并从前一相回收水相6和三恶烷,同时使后一相回流至反应区2.因此,三恶烷用作原料 通过简化的方法获得了高纯度和高收率的聚甲醛。
    • 4. 发明专利
    • Continuous polymerization of trioxane
    • 连续聚四氟乙烯
    • JPS59159812A
    • 1984-09-10
    • JP3179683
    • 1983-03-01
    • Asahi Chem Ind Co Ltd
    • MATSUZAKI KAZUHIKOMASAMOTO JIYUNZOU
    • C08G2/00C08G2/06C08G2/10C08G2/18
    • PURPOSE: To obtain continuously a high-quality polyacetal, by uniformly mixing, trioxane with a Lewis acid or mixing these with a cyclic ether under heating and feeding them maintained in a liquid phase to a polymerizer.
      CONSTITUTION: In the continuous polymerization for obtaining polyacetal by the homopolymerization of trioxane in the presence of a Lewis acid as a catalyst or the copolymerization of trioxane with a cyclic ether in the presence of the catalyst; the trioxane is mixed uniformly with the Lewis acid, or these are mixed uniformly with a cyclic ether at 64W140°C for 10W300sec, and the mixture maintained in a liquid phase is fed to a polymerizer. Preferably an agitator-mixer, static mixer, or double-shaft reactor is used. When an agitator-mixer is used, the distribution of a dwell time tends to be widened, so that it is preferred to use an agitator-mixer adapted to provide a sharp distribution of the dwell time.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:连续地获得高质量的聚缩醛,通过将三恶烷与路易斯酸均匀混合,或在加热下将其与环醚混合,并将它们保持在液相中供给聚合反应器。 构成:在路易斯酸作为催化剂的存在下,通过三恶烷的均聚获得聚缩醛的连续聚合,或者在催化剂存在下,三氧杂环己烷与环醚的共聚, 将三恶烷与路易斯酸均匀混合,或者将它们与环醚在64-140℃下均匀混合10-300秒,将保持在液相中的混合物加入到聚合反应器中。 优选使用搅拌器 - 混合器,静态混合器或双轴反应器。 当使用搅拌器 - 混合器时,停留时间的分布趋于变宽,因此优选使用适于提供停留时间的尖锐分布的搅拌器 - 混合器。
    • 5. 发明专利
    • Polyoxymethylene composition
    • 聚氧乙烯组合物
    • JPS59129247A
    • 1984-07-25
    • JP213683
    • 1983-01-12
    • Asahi Chem Ind Co Ltd
    • MATSUZAKI KAZUHIKOMASAMOTO JIYUNZOU
    • C08L59/00C08L77/00
    • PURPOSE: To provide a polyoxymethylene compsn. which reduces molding strains and has improved high cycle performance, consisting of a linear polyoxymethylene and a specified branched polyoxymethylene obtd. by polymerizing formaldehyde or trioxane.
      CONSTITUTION: A compsn. consists of a linear polyoxymethylene and a branched polyoxymethylene having a structure wherein an alkylene oxide is added to a polyhydric alcohol obtd. by polymerizing formaldehyde or trioxane in the presence of an adduct having at least three alcoholic hydroxyl groups per molecule or by copolymerizing formaldehyde or trioxane with a cyclic ether in the presence of said adduct. Preferred cyclic ethers are ethylene oxide, ethylene glycol formal and 1,4-butanediol formal from the viewpoint of improving the mechanical properties of the linear polyoxymethylene.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:提供聚甲醛组合物。 这降低了成型应变并且具有改善的高循环性能,由线性聚甲醛和特定的支化聚甲醛实例组成。 通过聚合甲醛或三恶烷。 宪法:一个公司 由线性聚甲醛和具有结构的支化聚甲醛组成,其中将环氧烷加入到多元醇类中。 在每分子具有至少三个醇羟基的加成物的存在下,或者在所述加合物的存在下,通过使甲醛或三恶烷与环醚共聚,来聚合甲醛或三恶烷。 从提高线性聚甲醛的机械性能的观点出发,优选的环状醚是环氧乙烷,乙二醇缩甲醛和1,4-丁二醇缩甲醛。
    • 6. 发明专利
    • Method of synthesizing trioxane in vapor phase
    • 在蒸气相中合成三氧化硫的方法
    • JPS5925387A
    • 1984-02-09
    • JP13363882
    • 1982-08-02
    • Asahi Chem Ind Co Ltd
    • MATSUZAKI KAZUHIKOMASAMOTO JIYUNZOU
    • C07D323/06B01J23/00B01J23/14B01J23/20B01J23/22B01J23/28B01J23/30B01J27/00B01J27/18C07B61/00
    • Y02P20/52
    • PURPOSE: To obtain the titled compound capable of giving high-molecular weight polyoxymethylene in high purity with little formation of by-products without depositing paraformaldehyde nor corroding apparatuses, by bringing formaldehyde in the vapor phase into contact with a heteropolyacid supported on a carrier.
      CONSTITUTION: A carrier, e.g. silica gel, is gently agitated in an aqueous solution of a heteropolyacid, e.g. phosphotungstic acid, at 80°C, and the carrier is then separated and dried at 120°C under reduced pressure to afford a catalyst containing the heteropolyacid supported on the carrier. The resultant catalyst is then packed in a stainless steel tube, etc. having a jacket, the stainless steel tube, etc. and brought into contact with the catalyst consisting of the heteropolyacid supported on the carrier and give the aimed trioxane of high purity.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:通过使气相中的甲醛与负载在载体上的杂多酸接触,获得能够以高纯度产生高分子量聚甲醛的标题化合物,几乎不形成副产物而不沉积多聚甲醛或腐蚀装置。 构成:载体,例如 硅胶,在杂多酸的水溶液中轻轻搅拌,例如 磷钨酸,在80℃下,然后将载体分离并在120℃下减压干燥,得到含载体载体上的杂多酸的催化剂。 然后将得到的催化剂装入具有夹套,不锈钢管等的不锈钢管等中,并与负载在载体上的杂多酸组成的催化剂接触,得到高纯度的目标三恶烷。