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    • 1. 发明专利
    • Production of xylylene glycol
    • 生产XYLYLENE GLYCOL
    • JPS59157039A
    • 1984-09-06
    • JP3036983
    • 1983-02-25
    • Mitsubishi Gas Chem Co Inc
    • YOSHINAKA SHIGEOTOKI TSUKASATSUJI TOMOJIUCHIYAMA SEIJI
    • C07C27/02C07C27/00C07C29/09C07C33/26C07C67/00
    • PURPOSE: To prepare the titled substance with little production of the condensation by product, by reacting xylylenediamine with a nitrous acid salt in the presence of a lower aliphatic carboxylic acid and water to obtain a mixture of the titled substance and its mono- and dicarboxylic acid ester, and hydrolyzing the ester.
      CONSTITUTION: Xylylenediamine is made to react with a nitrous acid salt (e.g. sodium nitrite) in the presence of a lower aliphatic carboxylic acid (preferably acetic acid) and water at 60W100°C to obtain a mixture of the titled substance and its mono- and dicarboxylic acid esters. The carboxylic acid is neutralized by adding an alkaline aqueous solution to the mixture, and the mixture is made alkaline with an alkali, hydrolyzed at 60W80°C under agitation, and treated with an organic solvent to extract the objective substance. The extraction residue composed mainly of sodium acetate is added with concentrated sulfuric acid to regenerate acetic acid at ≤25°C, and the acetic acid is recycled to the reaction system.
      EFFECT: The use of a large amount of acetic acid is not necessary, and the amount of waste water can be reduced.
      USE: A raw material of polyurethane, etc. or a modifier.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:为了制备产物缩合少的标题物质,在低级脂肪族羧酸和水的存在下,使苯二甲胺与亚硝酸盐反应,得到标题物质及其单羧酸和二羧酸的混合物 酯,并酯化。 构成:使甲苯二胺在低级脂族羧酸(优选乙酸)和水在60-100℃的存在下与亚硝酸盐(例如亚硝酸钠)反应,得到标题物质及其物质的混合物 单羧酸酯和二羧酸酯。 通过向混合物中加入碱性水溶液中和羧酸,并将混合物用碱碱化,在60-80℃搅拌下水解,并用有机溶剂处理以提取目标物质。 主要由乙酸钠组成的萃取残渣中加入浓硫酸,在<= 25℃再生乙酸,将乙酸再循环至反应体系。 效果:不需要使用大量的乙酸,可以减少废水量。 用途:聚氨酯等原料或改性剂。
    • 2. 发明专利
    • Production of xylylene glycol
    • 生产XYLYLENE GLYCOL
    • JPS59163331A
    • 1984-09-14
    • JP3680983
    • 1983-03-07
    • Mitsubishi Gas Chem Co Inc
    • YOSHINAKA SHIGEOTOKI TSUKASATSUJI TOMOJIUCHIYAMA SEIJI
    • C07C29/00C07C27/00C07C33/26C07C67/00
    • PURPOSE: To prepare the titled compound useful as a raw material or a modifying agent of polyurethane resin, etc., in high yield, in one step, suppressing the production of tarry material, by reacting xylylenediamine with a nitrous acid salt in the presence of a specific amount of water and a specific amount of a mineral acid.
      CONSTITUTION: High-purity xylylene glycol can be produced easily, by (1) mixinig 1mol of xylylenediamine, e.g. m- or p-xylylenediamine and a nitrous acid salt with 2.04W2.50 g-equivalent of hydrochloric acid or sulfuric acid at 0W100°C under agitation, (2) adding ≥8pts.wt. of water, based on 1pt.wt. of the xylylenediamine, to the system, (3) reacting the components at ≥70°C for 20min W5hr under normal pressure, (4) neutralizing the reaction mixture with an alkali after the completion of the reaction, and (5) separating the xylylene glycol from the product by conventional method. The molar ratio of the nitrous acid group/ xylylenediamine is preferably 2.0W2.5.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:为了制备用作原料的标题化合物或聚氨酯树脂等的改性剂,以高收率,一步法制备焦油物质,通过使苯二甲胺与亚硝酸盐反应,在 特定量的水和特定量的无机酸。 构成:可以容易地制备高纯度亚二甲苯基二醇,(1)将1mol苯二甲胺混合, m-或对苯二甲胺和亚硝酸盐,在0-100℃下,在2.0〜2.50g当量的盐酸或硫酸的搅拌下,(2)加入= 8pts.wt。 的水,基于1pt.wt。 (3)在常压下在> = 70℃下组分反应20分钟-5小时,(4)反应完成后用碱中和反应混合物,(5) 通过常规方法从产物中分离亚二甲苯基二醇。 亚硝酸基/苯二甲胺的摩尔比优选为2.0〜2.5。
    • 3. 发明专利
    • Preparation of dimethylethylamine
    • 二甲基胺的制备
    • JPS5942345A
    • 1984-03-08
    • JP15359882
    • 1982-09-03
    • Mitsubishi Gas Chem Co Inc
    • UCHIYAMA SEIJITSUJI TOMOJIYOSHINAKA SHIGEOTOKI TSUKASA
    • C07B61/00B01J23/00B01J23/80C07C67/00C07C209/00C07C209/26C07C211/05
    • Y02P20/52
    • PURPOSE: To obtain the titled substance useful as a catalyst for preparing polyurethane in high yield without deteriorating the catalytic activity nor side reactions, by reacting economical and advantageous acetaldehyde as a raw material with dimethylamine and hydrogen in the presence of a catalyst consisting of copper and zinc.
      CONSTITUTION: Acetaldehyde is reacted with dimethylamine and hydrogen in the presence of a catalyst consisting of copper and zinc or further one or more selected from zirconium, aluminum, barium, magnesium, molybdenum and manganese at 100W250°C under within ordinary pressure W15kg/cm
      2 .G, preferably ordinary pressure W10kg/cm
      2 .G reaction pressure range, to give the aimed compound. The content of the metal in the above-mentioned catalyst is preferably 40W80wt% copper and 7W50wt% zinc. The amount of the metal zirconium, etc. in the cocatalyst component is preferably 2W25wt%. 3W6mol dimethylamine and 3W6mol hydrogen are preferably used for 1mol acetaldehyde.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:为了获得标题物质,可用作催化剂,高产率地制备聚氨酯,而不会降低催化活性或副反应,通过使经济有利的乙醛作为原料与二甲胺和氢反应,在由铜和 锌。 构成:在100-250摄氏度的普通压力下,在由铜和锌组成的催化剂或更多的选自锆,铝,钡,镁,钼和锰中的一种或多种催化剂的存在下,乙醛与二甲基胺和氢气反应 - 15kg / cm 2,G,优选常压-10kg / cm 2 .G反应压力范围,得到目标化合物。 上述催化剂中金属的含量优选为40〜80重量%的铜和7〜50重量%的锌。 助催化剂成分中的金属锆等的含量优选为2〜25重量%。 3-6mol二甲胺和3-6mol氢优选用于1mol乙醛。
    • 4. 发明专利
    • Preparation of olefin
    • 烯烃的制备
    • JPS5759819A
    • 1982-04-10
    • JP13622080
    • 1980-09-30
    • Mitsubishi Gas Chem Co Inc
    • SUZUKI TAKASHIHASHIMOTO SHIYOUICHIROUNAKANO RIAKOTSUJI TOMOJI
    • C07C1/20B01J29/00B01J29/06C07B61/00C07C1/00C07C11/02C07C15/02C07C67/00
    • Y02P20/52Y02P30/42
    • PURPOSE: In preparing an olefin from methanol and/or dimethyl ether, to reduce the amount of a diluent used, to improve rate of reaction and selectivity, to prevent a catalyst from deteriorating, by reducing rate of feed of a raw material per crosssectional area of catalytic layer and per hour.
      CONSTITUTION: Using a catalyst comprising crystalline aluminosilicate zeolite (e.g., FZ-1 zeolite, etc.), olefin is prepared from methanol and/or dimethyl ether by a catalytic reactor of fixed bed. In the reaction, methanol and/or dimethyl ether are fed in amounts in range from 0.3W15g per sec per crosssectional area of catalyst, and the amount of a diluent used is reduced. The heat of reaction produced per crosssectional area of catalytic layer in a direction perpendicular to the direction of the raw material and per hour can be made small. The reduction in the amount of the feed of the diluent can save energy.
      COPYRIGHT: (C)1982,JPO&Japio
    • 目的:在从甲醇和/或二甲醚制备烯烃时,为了减少所用稀释剂的使用量,提高反应速率和选择性,防止催化剂变质,通过降低每个横截面积原料的进料速率 的催化层和每小时。 构成:使用包含结晶硅铝酸盐沸石(例如FZ-1沸石等)的催化剂,通过固定床的催化反应器由甲醇和/或二甲醚制备烯烃。 在该反应中,甲醇和/或二甲醚的供给量为每个催化剂横截面积为0.3-15g / sec,并且所用稀释剂的量减少。 在垂直于原料方向和每小时的方向上,催化剂层的每个横截面产生的反应热可以减小。 稀释剂进料量的减少可以节省能源。
    • 5. 发明专利
    • Method for producing xylylene glycol
    • 生产XYLYLENE GLYCOL的方法
    • JPS59163332A
    • 1984-09-14
    • JP3681083
    • 1983-03-07
    • Mitsubishi Gas Chem Co Inc
    • YOSHINAKA SHIGEOTOKI TSUKASATSUJI TOMOJIUCHIYAMA SEIJI
    • C07C29/09C07C27/00C07C29/00C07C33/26C07C67/00
    • C07C29/00C07C33/26
    • PURPOSE: To prepare the titled compound useful as a raw material of polyurethane resin, etc. in high yield, in one step, suppressing the production of tarry material, by reacting xylylenediamine with a nitrous acid salt in the presence of a specific amount of water and a mineral acid within a specific pH range.
      CONSTITUTION: High-purity xylylene glycol can be prepared, easily, in high yield, by (1) mixing 1pt.wt. of xylylenediamine such as m- or p-xylylenediamine with ≥5pts.wt. of water and a mineral acid of an amount to keep the pH of the reaction system at 1.5W5.0, at 0W100°C under stirring, (2) reacting the components in the presence of a nitrous acid salt at ≥70°C for 20minW5hr under normal pressure, (3) neutralizing the reaction mixture with an alkali after the completion of the reaction, and (4) separating the xylylene glycol from the product by conventional method. The amount of the nitrous acid salt is selected preferably to give the molar ratio of the nitrous acid group/xylylenediamine of 2.0W2.5.
      COPYRIGHT: (C)1984,JPO&Japio
    • 目的:通过在特定量的水存在下,使苯二甲胺与亚硝酸盐反应,以高产率制备用作聚氨酯树脂等原料的标题化合物,一步法抑制焦油物质的生成 和特定pH范围内的无机酸。 构成:高纯度亚二甲苯可以容易地以高产率制备,(1)混合1pt.wt. 的苯二甲胺如m-对苯二甲胺,其中> = 5pts.wt。 的水和无机酸,其量为在0-100℃下在搅拌下将反应体系的pH保持在1.5-5.0,(2)在亚硝酸盐存在下使组分反应为> 70 在常压下反应20分钟-5小时,(3)反应完成后用碱中和反应混合物,和(4)通过常规方法从产物中分离亚二甲苯基二醇。 优选选择亚硝酸盐的量以使亚硝酸基/苯二甲胺的摩尔比为2.0-2.5。
    • 6. 发明专利
    • Preparation of lower olefin
    • 低烯烃的制备
    • JPS5767526A
    • 1982-04-24
    • JP14258180
    • 1980-10-13
    • Mitsubishi Gas Chem Co Inc
    • SUZUKI TAKASHIHASHIMOTO SHIYOUICHIROUNAKANO RIAKOTSUJI TOMOJI
    • C10G3/00B01J29/00B01J29/06C07B61/00C07C1/00C07C1/20C07C1/32C07C11/02C07C67/00
    • Y02P20/52Y02P30/42
    • PURPOSE: To obtain a lower olefin in a high rate of reaction and selectivity with the slight deterioration of a catalyst and high partial pressure of raw materials, by reacting methanol with dimethyl ether in a substance, e.g. n-heptane, having a specific heat capacity as a diluting agent in the presence of a specific catalyst.
      CONSTITUTION: Methanol is reacted with dimethyl ether in the presence of a catalyst, having a spacing and relative intensity as shown in the table in the X-ray diffraction pattern, and containing a crystalline aluminosilacate with or without fluorine to give a lower olefin. In the process, the raw materials are diluted witha substance having a specific molar heat ≥100Joul.K
      -1 at a constant pressure and 600° K and oridinary pressure, e.g. a 3W7C straight chain saturated hydrocarbon such as propane or n-pentane, and the reaction is carried out. The high partial pressure of the raw materials provides the energy saving.
      COPYRIGHT: (C)1982,JPO&Japio
    • 目的:通过使甲醇与二甲醚在物质如甲醇中反应,以高反应速率和选择性获得低级烯烃,催化剂的轻微劣化和原料的高分压。 正庚烷,在特定催化剂存在下具有作为稀释剂的比热容。 构成:在催化剂存在下,甲醇与X射线衍射图中所示的间隔和相对强度反应,并含有具有或不具有氟的结晶铝硅酸盐,得到低级烯烃。 在此过程中,原料在一定压力和600度下用特定摩尔热> = 100Joul.K -1的物质稀释。 K和压力,例如 3-7C直链饱和烃如丙烷或正戊烷,并进行反应。 原料的高分压提供节能。