Continuous preparation of cyclohexanone oxime
    1.
    发明授权
    Continuous preparation of cyclohexanone oxime 失效
    CYCLOHEXANONE OXIME连续制备

    公开(公告)号:US3862230A

    公开(公告)日:1975-01-21

    申请号:US42271273

    申请日:1973-12-07

    Applicant: STAMICARBON

    Abstract: A process for the continuous preparation of an oxime from cyclohexanone and an aqueous buffered solution of a hydroxylammonium salt together with free phosphoric acid, phosphates, nitrates, and optionally sulphates all in controlled amounts and without the use of an organic solvent is disclosed. The resulting aqueous reaction mixture contains a manageable amount of unreacted cyclohexanone which is subsequently recovered and recirculated.

    Abstract translation: 公开了一种从环己酮和羟基铵盐连续制备肟的方法以及游离磷酸,磷酸盐,硝酸盐和任选的硫酸盐,其全部以受控量和不使用有机溶剂。 所得的含水反应混合物含有可处理量的未反应的环己酮,随后回收并再循环。

    Process for recovery of {68 -caprolactam from a reaction mixture of {68 -caprolactam and sulphuric acid
    3.
    发明授权
    Process for recovery of {68 -caprolactam from a reaction mixture of {68 -caprolactam and sulphuric acid 失效
    从{68-己内酰胺和硫酸的反应混合物中回收{68-己内酰胺的方法

    公开(公告)号:US3907781A

    公开(公告)日:1975-09-23

    申请号:US48260174

    申请日:1974-06-24

    Applicant: STAMICARBON

    CPC classification number: C07D201/16 E05Y2900/104

    Abstract: Epsilon -CAPROLACTAM IS RECOVERED FROM A Beckmann rearrangement mixture of the lactam and aqueous sulfuric acid by simultaneously neutralizing the rearrangement mixture with ammonia at a pressure of 1-5 atmospheres and crystallizing out ammonium sulfate, the heat liberated by the neutralization reaction is removed from the system by evaporating a portion of the water from the solution. At the conditions employed hydrolysis of the lactam is substantially reduced if not entirely avoided.

    Abstract translation: 通过在1-5个大气压的压力下同时用氨中和重排混合物并结晶出硫酸铵,将ε-CAPROLACTAM从内酰胺和硫酸水溶液的贝克曼重排混合物中回收,中和反应释放的热量从 系统通过从溶液中蒸发一部分水。 在使用条件下,如果不完全避免,内酰胺的水解将显着降低。

    RECOVERY OF EPSILON-CAPROLACTAM
    5.
    发明专利

    公开(公告)号:AU7072774A

    公开(公告)日:1976-01-08

    申请号:AU7072774

    申请日:1974-07-02

    Applicant: STAMICARBON

    Abstract: epsilon -CAPROLACTAM IS RECOVERED FROM A Beckmann rearrangement mixture of the lactam and aqueous sulfuric acid by simultaneously neutralizing the rearrangement mixture with ammonia at a pressure of 1-5 atmospheres and crystallizing out ammonium sulfate, the heat liberated by the neutralization reaction is removed from the system by evaporating a portion of the water from the solution. At the conditions employed hydrolysis of the lactam is substantially reduced if not entirely avoided.

    10.
    发明专利
    未知

    公开(公告)号:DE1263722B

    公开(公告)日:1968-03-21

    申请号:DEST022773

    申请日:1964-10-05

    Applicant: STAMICARBON

    Abstract: An aqueous solution containing both phosphoric and nitric acids is extracted with a poorly water-miscible aliphatic ketone or ether having from 4 to 13 carbon atoms, the concentration of the starting solution and the weight ratio of the starting solution to the extracting agent being selected so that at least 90% of the nitric acid but not more than 10% of the phosphoric acid passes into the organic phase. The starting solution preferably contains at least 40%, but not more than 75%, by weight of water. When the starting solution contains from 40% to 70% by weight of water, the weight ratio between the acid solution and the ketone or ether preferably is kept at from 1: 1 to 1: 3, a higher proportion of extracting agent being favoured for more dilute solutions. The extraction either may be performed batchwise in one or a plurality of stages or may be carried out continuously with countercurrent flow of extracting agent and acid solution. The ketone or ether may be diethyl ether, diisopropyl ether, dibutyl ether, diisoamyl ether, methyl-isobutyl ketone, methyl-isoamyl ketone, butyl-ethyl ketone, diisobutyl ketone or dibutyl carbitol; the preferred extracting agent is methyl-isobutyl ketone. The above separation process may be applied in the recovery of phosphoric acid from the liquor resulting from the decomposition of phosphate rock by concentrated nitric acid. Such a procedure, an example of which is fully described and illustrated in the Specification, may entail preparing an aqueous solution of phosphoric and nitric acids by decomposing phosphate rock with nitric acid having a concentration of at least 45% by weight acid, lowering the molar calcium oxide/phosphorus pentoxide ratio of the solution to below 1.5 by cooling to remove calcium nitrate, subjecting the solution to an extraction with a butyl or amyl alcohol, freeing the resulting acids-containing organic extract from residual calcium nitrate by washing with a solution containing phosphoric acid and possibly nitric acid and having a concentration of at least 25% by weight total acid(s), washing the acid-washed organic extract with water in an amount such that not more than three quarters of the total acids present passes from the organic extract to the water, and separating the phosphoric acid from the nitric acid in the resulting aqueous acid solution by the extraction process described previously.

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