Preparation of .epsilon.-caprolactone
    1.
    发明授权
    Preparation of .epsilon.-caprolactone 失效
    ε-己内酯的制备

    公开(公告)号:US4341709A

    公开(公告)日:1982-07-27

    申请号:US150260

    申请日:1980-05-15

    CPC分类号: C07D315/00

    摘要: A process for the preparation of .epsilon.-caprolactone comprising:(a) reacting cyclohexanone with a solution of perpropionic acid in an organic solvent at a molar ratio of cyclohexanone;perpropionic acid of about 1.1-5:1 at a temperature of about 10.degree. to 80.degree. C. to form a reaction mixture consisting essentially of .epsilon.-caprolactone, propionic acid and organic solvent,(b) distilling the reaction mixture from (a) in a first distillation unit to obtain a distillate comprising the organic solvent and a distillation residue,(c) introducing the distillation residue from (b) at a point into a second distillation unit to obtain a distillate comprising propionic acid and unreacted cyclohexanone, removing from the second distillation unit, separately from one another and at a point below the point of introduction into the second distillation unit, .epsilon.-caprolactone and any high-boiling constituents, and,(d) distilling in a third distillation unit the distillate from (c) to obtain a distillate consisting essentially of propionic acid and a distillation residue comprising a mixture of propionic acid and cyclohexanone.

    摘要翻译: 一种制备ε-己内酯的方法,包括:(a)使环己酮与过丙酸在有机溶剂中的溶液以环己酮的摩尔比约1.1-5:1的约0.1〜5:1的摩尔比在约10℃〜 形成基本上由ε-己内酯,丙酸和有机溶剂组成的反应混合物,(b)在第一蒸馏单元中将反应混合物从(a)中蒸馏,得到包含有机溶剂和蒸馏残余物的馏出物 (c)在一点将来自(b)的蒸馏残余物引入第二蒸馏单元以获得包含丙酸和未反应的环己酮的馏出物,从第二蒸馏单元彼此分离并在低于 引入第二蒸馏装置,ε-己内酯和任何高沸点组分,和(d)在第三蒸馏装置中蒸馏出馏出物(c)得到 基本上由丙酸组成的馏出物和包含丙酸和环己酮的混合物的蒸馏残渣。

    Process for the production of solutions or suspensions of cyanuric
chloride in aqueous organic solvents
    3.
    发明授权
    Process for the production of solutions or suspensions of cyanuric chloride in aqueous organic solvents 失效
    用于生产氰尿酰氯在含水有机溶剂中的溶液或悬浮液的方法

    公开(公告)号:US4017413A

    公开(公告)日:1977-04-12

    申请号:US632952

    申请日:1975-11-18

    IPC分类号: C07D251/28 B01F3/08

    CPC分类号: C07D251/28

    摘要: There is provided a process for the production of a solution or suspension of cyanuric chloride in a water containing organic solvent wherein the liquid cyanuric chloride and the organic-aqueous solvent are mixed together while being agitated, the liquid cyanuric chloride at a temperature between its melting point and 200.degree. C. is led into the flowing organic-aqueous solvent with a velocity of Vcy (in kg per hour) wherein ##EQU1## where P is the desired concentration of cyanuric chloride in the solution or suspension to be produced in weight %, P.sub.LM is the concentration of cyanuric chloride in the solvent used which also includes O,V.sub.lm is the velocity of the solvent added in kg/h,And P.sub.LM, V.sub.LM and T.sub.LM, the temperature of the added solvent, are so selected that the expression ##EQU2## does not exceed the boiling temperature in .degree. C. of the solvent used and wherein C.sub.p (LM) and C.sub.p (Cy) signify the specific heat capacities in cal. x g.sup.-.sup.1 .times. (.degree.degree C).sup.-.sup.1 of the solvent and cyanuric chloride respectively, whereupon in a given case within at most 3 minutes after bringing the cyanuric chloride and solvent into contact the flowing mixture is cooled to the desired storage temperature.

    摘要翻译: 提供了一种在含有有机溶剂的水中制备氰尿酰氯的溶液或悬浮液的方法,其中液体氰尿酰氯和有机 - 水溶剂在搅拌下混合在一起,液态氰尿酰氯在其熔融 点和200℃以Vcy速度(以kg /小时计)流入有机 - 水溶剂,其中P是待生成的溶液或悬浮液中所需浓度的氰尿酰氯,其重量% PLM是所用溶剂中氰尿酰氯的浓度,其还包括O,VLM是以kg / h加入的溶剂的速度,而PLM,VLM和TLM,加入的溶剂的温度如此选择,使得表达式 &lt; IMAGE&gt;不超过使用的溶剂的沸点(℃),其中Cp(LM)和Cp(Cy)表示比热容。 xg <1>(℃C)-1的溶剂和氰尿酰氯,因此在给出的情况下,在将氰尿酰氯和溶剂接触之前的最多3分钟内,将流动的混合物冷却至所需的 储存温度。

    Working up of the residual gases resulting from the production of
cyanuric chloride
    4.
    发明授权
    Working up of the residual gases resulting from the production of cyanuric chloride 失效
    处理由产生氰尿酰氯产生的残留气体

    公开(公告)号:US4434148A

    公开(公告)日:1984-02-28

    申请号:US81555

    申请日:1979-10-03

    CPC分类号: C01C3/004 C07D251/28

    摘要: The residual gases obtained in the production of cyanuric chloride having a pressure of 1-5 bar (absolute) preferably 1-4 bar, are worked up by leading them into the lower portion of a column, reacted in the column with at least the equivalent amount of hydrogen cyanide to form cyanogen chloride and led in countercurrent flow to the water charged to the upper portion of the column whereupon the aqueous solution of cyanogen chloride formed is withdrawn from the lower portion of the column and preferably is returned into the production portion of the plant for recovery of the cyanogen chloride while the purified waste gas of the column leaves in the upper portion of the column.

    摘要翻译: 在生产具有1-5巴(绝对)压力优选1-4巴的压力的氰尿酰氯中获得的残余气体通过将它们引入塔的下部来处理,在塔中反应至少具有相当于 氰化氢的量以形成氯化氰,并且逆流地流向加到塔上部的水,由此形成的氯化氢水溶液从柱的下部排出,优选返回到 用于回收氯化氰的设备,而塔的净化废气在塔的上部离开。

    Process for the production of hydrogen cyanide
    5.
    发明授权
    Process for the production of hydrogen cyanide 失效
    生产氰化氢的方法

    公开(公告)号:US4387081A

    公开(公告)日:1983-06-07

    申请号:US304049

    申请日:1981-09-21

    IPC分类号: B01J23/00 C01C3/02

    CPC分类号: C01C3/0233

    摘要: In order to be independent of the situation in regard to methane and natural gas and at the same time to obtain a heating gas there is employed in the hydrocyanic acid-methane-ammonia process (the BMA process) in place of methane an alkanol or alkanediol having 2-4 carbon atoms, preferably ethyl alcohol, and this is reacted with ammonia in a C:N ratio of 0.8:1 to 2:1. Optionally additional hydrogen can be present.

    摘要翻译: 为了独立于甲烷和天然气的情况,同时获得加热气体,采用氢氰酸 - 甲烷 - 氨法(BMA法)代替烷烃或链烷二醇 具有2-4个碳原子,优选乙醇,并且其与C:N比为0.8:1至2:1的氨反应。 可选地,可以存在另外的氢。

    Process for isolating propylene glycol diesters in the preparation of
propylene oxide
    6.
    发明授权
    Process for isolating propylene glycol diesters in the preparation of propylene oxide 失效
    在制备环氧丙烷中分离丙二醇二酯的方法

    公开(公告)号:US4159925A

    公开(公告)日:1979-07-03

    申请号:US858319

    申请日:1977-12-09

    摘要: Process for isolating propylene glycol diacarboxylates in the preparation of propylene oxide by reaction of propylene with a solution of percarboxylic acid in an organic solvent, the boiling point of which is lower than that of the carboxylic acid which corresponds to the percarboxylic acid used as the epoxidizing agent, and higher than that of propylene oxide, separation, by distillation, of the reaction mixture which essentially contains propylene oxide, the carboxylic acid corresponding to the percarboxylic acid used as the epoxidizing agent and one or more of the by-products propyleneglycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate as well as propylene and the organic solvent, into a fraction containing propylene oxide and propylene and a fraction containing the carboxylic acid, the by-products mentioned and the organic solvent and further separation of the fractions into the individual components by distillation. The fraction containing the carboxylic acid, one or more of the by-products propylene glycol, propylene glycol monocarboxylate and propylene glycol dicarboxylate, and the organic solvent is distilled in a column at pressures of 1.5 to 6 bars and with an average residence time of 10 to 90 minutes in the sump. The organic solvent is removed as the top product and the carboxylic acid and the corresponding propylene glycol dicarboxylate is obtained as the sump product. From the sump product the propylene glycol dicarboxylate is isolated in a manner which is in itself known.

    摘要翻译: 通过丙烯与过羧酸在有机溶剂中的溶液反应制备环氧丙烷中的丙二醇二羧酸盐的分离方法,其沸点低于对应于用作环氧化物的过羧酸的羧酸 试剂,高于环氧丙烷,通过蒸馏分离基本上含有环氧丙烷的反应混合物,对应于用作环氧化剂的过羧酸的羧酸和一种或多种副产物丙二醇,丙烯 乙二醇单羧酸酯和丙二醇二羧酸酯以及丙烯和有机溶剂转化成含有环氧丙烷和丙烯的馏分和含有羧酸的馏分,所述副产物和有机溶剂,并将馏分进一步分离成单独组分 通过蒸馏。 将含有羧酸,一种或多种副产物丙二醇,丙二醇单羧酸酯和丙二醇二羧酸酯和有机溶剂的级分在1.5至6巴的压力下在柱中蒸馏,并且平均停留时间为10 在水槽中90分钟。 作为顶部产物除去有机溶剂,得到羧酸和相应的丙二醇二羧酸酯作为贮槽产物。 从贮槽产品中,以本身已知的方式分离丙二醇二羧酸酯。

    Process of making penicillamine
    7.
    发明授权
    Process of making penicillamine 失效
    制作青霉胺的过程

    公开(公告)号:US4061674A

    公开(公告)日:1977-12-06

    申请号:US657605

    申请日:1976-02-12

    IPC分类号: C07D277/06 C07C99/00

    CPC分类号: C07D277/06

    摘要: Penicillamine or a homolog thereof is obtained by reacting a 2-disubstituted-5,5-alkyl-thiazolidine nitrile, alkyl having 1 to 6 carbon atoms, with a mineral acid in a two-stage proceeding wherein in the first stage relatively low temperatures and a relatively high concentration of the mineral acid are employed while in the second stage the concentration of the acid is relatively low and the temperatures are relatively high, the term "relatively" referring to the relationship of said two stages of the reaction with mineral acid.

    摘要翻译: 青霉胺或其同系物是通过2-二取代-5,5-烷基 - 噻唑烷腈,具有1至6个碳原子的烷基与无机酸反应得到的,其中在两阶段进行,其中在第一阶段相对低的温度和 使用相对高浓度的无机酸,而在第二阶段酸的浓度相对较低并且温度相对较高,术语“相对”是指反应两个阶段与无机酸的关系。

    Process for the production of pure racemic acid and mesotartaric acid
    8.
    发明授权
    Process for the production of pure racemic acid and mesotartaric acid 失效
    制备纯外消旋酸和甲磺酸的方法

    公开(公告)号:US4048225A

    公开(公告)日:1977-09-13

    申请号:US660789

    申请日:1976-02-24

    摘要: Pure racemic acid (dl-tartaric acid) and meso tartaric acid are produced by reaction of an alkali maleate with aqueous hydrogen peroxide in the presence of a catalyst which is an alkali molybdate or a mixture of an alkali molybdate and alkali tungstate in a process wherein the molar ratio of hydrogen peroxide to maleic acid is greater than 1:1 and the alkali salt of cis-epoxysuccinic acid formed together with the catalyst in a given case after destroying the excess hydrogen peroxide and other peroxygen compounds, are converted to free cis-epoxysuccinic acid and free molybdic acid or mixture of free molybdic acid and free tungstic acid by leading them over a strongly acidic cation exchanger, whereupon the hydrolysis of the free cis-epoxysuccinic acid to racemic acid and meso-tartaric acid can take place either in the presence of or the absence of the free molybdic acid or mixture of free molybdic acid and free tungstic acid, whereby the catalyst in the case of catalyst free hydrolysis before, and in the case of catalyst containing hydrolysis after this hydrolysis is removed with an anion exchanger and the racemic acid is then in known manner crystallized out of the catalyst free hydrolysis mixture by lowering the temperature in a given case with evaporation of water, whereupon the meso-tartaric acid remains in the mother liquor, and there is recovered from the mother liquor either by crystallization or by evaporation to dryness, in a given case in admixture with racemic acid, unreacted cis-epoxysuccinic acid and maleic acid, while the anion exchanger laden with the molybdic acid or mixture of molybdic acid and tungstic acid is regenerated in known manner with dilute aqueous alkali and, in a given case, the resulting solution of alkali molybdate or mixture of alkali molybdate and alkali tungstate, eventually after treatment with activated carbon is returned directly into the epoxidation step.

    摘要翻译: 通过碱金属马来酸盐与过氧化氢水溶液在催化剂的存在下,在碱金属钼酸盐或碱金属钼酸盐和碱金属钨酸盐的混合物存在下,制备纯外消旋酸(dl-酒石酸)和内消旋酒石酸, 过氧化氢与马来酸的摩尔比大于1:1,而在过去的过氧化氢和其他过氧化合物破坏之后,在给定情况下与催化剂一起形成的顺式环氧琥珀酸的碱式盐转化为游离的顺式 - 环氧琥珀酸和游离钼酸或游离钼酸和游离钨酸的混合物通过引导它们在强酸性阳离子交换剂上,由此将游离顺式 - 环氧琥珀酸水解成外消旋酸和内消旋酸 - 酒石酸可以在 存在或不存在游离钼酸或游离钼酸和游离钨酸的混合物,从而在催化剂自由水解的情况下催化剂b 之前,并且在用水解阴离子交换剂除去水解后的催化剂的情况下,然后以已知的方式将外消旋酸从无催化剂的水解混合物中结晶出来,在给定的情况下通过降低水的温度在水中蒸发, 中间酒石酸保留在母液中,通过结晶或通过蒸发至干,从母液中回收,在给定情况下与外消旋酸,未反应的顺式 - 环氧琥珀酸和马来酸混合,而阴离子 以钼酸或钼酸和钨酸的混合物的交换剂以已知的方式用稀碱水再生,在给定情况下,所得到的钼酸碱盐或钼酸碱盐和碱金属钨酸盐的混合物最终经活化后处理 碳直接返回到环氧化步骤中。

    Process for the production of cyanogen chloride using hydrogen peroxide
with pressure
    9.
    发明授权
    Process for the production of cyanogen chloride using hydrogen peroxide with pressure 失效
    使用过氧化氢压力生产氯化氰的方法

    公开(公告)号:US4046862A

    公开(公告)日:1977-09-06

    申请号:US684352

    申请日:1976-05-07

    IPC分类号: C01C3/00 C01B21/18

    CPC分类号: C01C3/004 Y02P20/584

    摘要: Cyanogen chloride or cyanogen bromide is prepared by reaction of hydrogen cyanide with hydrogen chloride or hydrochloric acid (or hydrogen bromide or hydrobromic acid) and hydrogen peroxide in aqueous medium in the presence of cupric and ferric ions under superatmospheric pressure, preferably between 1.5 and 16 bar, and the cyanogen chloride (or cyanogen bromide) recovered separated from oxygen and nitrogen. In a preferred form of the invention, the hydrogen chloride or hydrochloric acid is either partially or entirely formed directly in the recycling catalyst solution of cupric and ferric ions by reaction of chlorine and hydrogen cyanide, either with or without pressure.

    摘要翻译: 在高于大气压下,优选在1.5至16巴之间,在铜和铁离子存在下,将氰化氢与氯化氢或盐酸(或溴化氢或氢溴酸)和过氧化氢在水介质中反应制备氯化氰或溴化氰 ,并从氧和氮分离回收的氯化氰(或溴化氰)。 在本发明的优选形式中,氯化氢或盐酸通过氯气和氰化氢的反应,在或不加压力下,直接在铜和铁离子的再循环催化剂溶液中部分或完全形成。

    Continuous process for recovery of glycide
    10.
    发明授权
    Continuous process for recovery of glycide 失效
    持续的糖苷还原过程

    公开(公告)号:US4009188A

    公开(公告)日:1977-02-22

    申请号:US551015

    申请日:1975-02-19

    CPC分类号: C07D301/32

    摘要: Glycide is prepared by reacting allyl alcohol with hydrogen peroxide in the presence of a tungsten compound as a catalysts the excess allyl alcohol and the greatest part of the water distilled off, the sump mixture obtained in the distillation is split at 110.degree.-220.degree. C. and 5 to 60 torr in a thin layer evaporator into a volatile portion which is predominantly glycide, high boiling by products and the residual part of the water and a sump portion of glycerine, polyglycerine and catalysts. The volatile liquid portion is broken into glycide, water and high boiling byproducts at 5 to 60 torr in a distillation apparatus directly connected to the thin layer evaporator.

    摘要翻译: 通过使烯丙醇与过氧化氢在钨化合物作为催化剂存在下制备过量的烯丙醇和蒸馏出的最大部分水,将蒸馏中获得的集水器混合物在110°-220℃ 和5至60托在薄层蒸发器中成为挥发性部分,其主要是糖苷,产物高沸点,剩余部分水和甘油,聚甘油和催化剂的贮槽部分。 在与薄层蒸发器直接连接的蒸馏装置中,挥发性液体部分在5至60托下破碎为糖,水和高沸点副产物。