VERFAHREN ZUR KONTINUIERLICHEN HERSTELLUNG VON ADIPODINITRIL
    1.
    发明申请
    VERFAHREN ZUR KONTINUIERLICHEN HERSTELLUNG VON ADIPODINITRIL 审中-公开
    方法用于连续生产己二腈

    公开(公告)号:WO2016041930A1

    公开(公告)日:2016-03-24

    申请号:PCT/EP2015/071031

    申请日:2015-09-15

    Applicant: BASF SE

    Abstract: Beschrieben wird ein Verfahren zur kontinuierlichen Herstellungvon Adipodinitril durch Hydrocyanierung von 3-Pentennnitril, bei dem man a) 3-Pentennitril hydrocyaniert unter Erhalt eines Reaktionsaustrags, der Adipodinitril enthält, b) in einer Aufarbeitung 1 aus dem Reaktionsaustrag des Reaktors R1 in einer ersten Destillationsvorrichtung als Kopfprodukt ein Gemisch enthaltend cis-2-Methyl-2- butennitril und cis-2-Pentennitril abtrennt, c) das Gemisch enthaltend cis-2-Methyl-2-butennitril und cis-2-Pentennitril aus Schritt b) in einem Reaktor R2 in Gegenwart von Aluminiumoxid als Katalysator kontinuierlich zu einem 3-Pentennitril enthaltenden Produktgemisch isomerisiert, d)aus dem Reaktionsaustrag des Reaktors R2 in einer Aufarbeitung 2 in einer Destillationsvorrichtung cis-2-Methyl-2-butennitril als Kopfprodukt abtrennt und ausschleust.

    Abstract translation: 公开了一种用于通过3-戊烯腈的氢氰化连续制备己二腈的方法,其中a)3-戊烯腈氢氰化,得到含有反应产物混合物己二腈,b)以进行后处理1为从反应器R1的反应流出物在第一蒸馏装置 塔顶产物含有顺式-2-甲基-2-丁烯腈和顺式-2-戊烯腈的混合物被分离出来,c)含顺式-2-甲基-2-丁烯腈和来自步骤b顺式-2-戊烯腈)在反应器R2中的混合物 氧化铝的存在下连续异构化成含3-戊烯腈产物混合物作为催化剂,d)从所述反应器R2的反应流出物中分离在一个工作式2在蒸馏设备中顺式-2-甲基-2-丁烯腈作为顶部产物和ausschleust。

    INTEGRATED PROCESS FOR NITRILE MANUFACTURE WITH ENHANCED LIQUID-LIQUID EXTRACTION
    2.
    发明申请
    INTEGRATED PROCESS FOR NITRILE MANUFACTURE WITH ENHANCED LIQUID-LIQUID EXTRACTION 审中-公开
    具有增强液体萃取的氮化物制造的综合工艺

    公开(公告)号:WO2015200630A1

    公开(公告)日:2015-12-30

    申请号:PCT/US2015/037686

    申请日:2015-06-25

    Abstract: Phosphorus-containing ligands are recovered from mixtures comprising 3-pentenenitrile (3PN) and adiponitrile (ADN), using liquid-liquid extraction. ADN is produced by hydrocyanation of 3PN. The ADN is hydrogenated to produce a hexamethyiene diamine (HMD) and at Ieast one byproduct including bis-hexamethylene triamine (BHMT) or 1,2-diaminocyclohexane. At Ieast a portion of the HMD product or byproduct is used to enhance the liquid-liquid extraction to recover phosphorus-containing ligand.

    Abstract translation: 使用液 - 液萃取从含有3-戊烯腈(3PN)和己二腈(ADN)的混合物中回收含磷配体。 ADN由3PN的氢化生成。 将ADN氢化以产生六甲基二胺(HMD),并在Ieast一种副产物包括双 - 六亚甲基三胺(BHMT)或1,2-二氨基环己烷。 在Ieast,HMD产物或副产物的一部分用于增强液 - 液萃取以回收含磷配体。

    PROCESS FOR STABILIZING HYDROCYANATION CATALYST
    3.
    发明申请
    PROCESS FOR STABILIZING HYDROCYANATION CATALYST 审中-公开
    稳定化学催化剂的方法

    公开(公告)号:WO2013181096A1

    公开(公告)日:2013-12-05

    申请号:PCT/US2013/042640

    申请日:2013-05-24

    Abstract: The invention provides a method of forming a phosphonate diester compound from a ligand hydrolysis product (LHP) of a phosphite ligand used in a nickel-phosphite hydrocyanation catalyst, such as for conversion of 3-pentenenitrile to adiponitrile, which serves to eliminate acidic LHP compound for a hydrocyanation reaction milieu where the acidic LHP can catalyze further catalyst ligand destruction. The invention further provides phosphonate disester compounds prepared by alkylation of diarylphosphite LHP in the presence of a nickel-phosphite catalyst comprising a bidentate ligand, and a continuous hydrocyanation process for production of adiponitrile wherein catalyst ligand breakdown is inhibited through inactivation of ligand hydrolysis products towards further breakdown. A method of stabilizing a hydrocyanation catalyst is provided.

    Abstract translation: 本发明提供了一种由亚磷酸氢氰化催化剂中使用的亚磷酸酯配体的配位体水解产物(LHP)形成膦酸二酯化合物的方法,例如用于将3-戊烯腈转化成己二腈,其用于消除酸性LHP化合物 对于氢化反应环境,其中酸性LHP可以催化另外的催化剂配体破坏。 本发明还提供了在含有二齿配位体的亚磷酸二氢镍催化剂的存在下烷基化亚磷酸二氢钠LHP制备的膦酸酯二酯化合物,以及用于生产己二腈的连续氢氰化方法,其中通过使配体水解产物失活进一步抑制催化剂配体分解 分解。 提供了一种稳定氢氰化催化剂的方法。

    NOVEL PROCESS FOR THE MANUFACTURE OF METHYL LIMONITRILE
    4.
    发明申请
    NOVEL PROCESS FOR THE MANUFACTURE OF METHYL LIMONITRILE 审中-公开
    用于制造甲基硫酸钠的新工艺

    公开(公告)号:WO2013120808A1

    公开(公告)日:2013-08-22

    申请号:PCT/EP2013/052689

    申请日:2013-02-11

    CPC classification number: C07C253/10 C07C253/30 C07C253/34 C07C255/07

    Abstract: The present invention is directed to a process for the manufacture of methyl limonitrile comprising a mixture of 3,7-dimethyl-2,6-nonadiene nitrile, 3,7-dimethyl-3,6-nonadiene nitrile and 7-methyl-3-methylene-6-nonene nitrile comprising the following steps: a) reacting 6-methyl-5-octen-2-one with cyano acetic acid and removing carbon dioxide and water, wherein the reaction and the removal of carbon dioxide and water are performed in the presence of a base and a co-base 1 in an organic solvent, and wherein the organic solvent is a solvent which forms a heteroazeotrop with water; b) removing the solvent and the base of the reaction mixture obtained after having performed step a) or step c) by distillation to obtain a reaction mixture, whereby this step may optionally be performed in the presence of a co-base 2; c) isomerizing the reaction mixture obtained after having performed step a) or step b) to obtain an isomerized reaction mixture in the presence of a co-base 2; whereby step b) can be performed before or after step c).

    Abstract translation: 本发明涉及一种制备甲基有限公司的方法,该方法包括3,7-二甲基-2,6-壬二烯腈,3,7-二甲基-3,6-壬二烯腈和7-甲基-3- 亚甲基-6-壬烯腈包括以下步骤:a)使6-甲基-5-辛烯-2-酮与氰基乙酸反应并除去二氧化碳和水,其中二氧化碳和水的反应和除去在 在有机溶剂中存在碱和共碱1,其中有机溶剂是与水形成杂合性的溶剂; b)通过蒸馏除去在进行步骤a)或步骤c)之后获得的反应混合物的溶剂和碱,得到反应混合物,由此该步骤可任选地在共碱2存在下进行; c)使在步骤a)或步骤b)中获得的反应混合物异构化,以在共碱2存在下得到异构化反应混合物; 由此步骤b)可以在步骤c)之前或之后进行。

    PROCESS FOR MAKING NITRILES
    6.
    发明申请
    PROCESS FOR MAKING NITRILES 审中-公开
    制造NITRILES的工艺

    公开(公告)号:WO2012005911A1

    公开(公告)日:2012-01-12

    申请号:PCT/US2011/040651

    申请日:2011-06-16

    CPC classification number: C07C253/10 Y02P20/584 C07C255/04

    Abstract: Adiponitrile is made by reacting 3-pentenenitrile with hydrogen cyanide. The 3- pentenenitrile is made by reacting 1,3-butadiene with hydrogen cyanide. The catalyst for the reaction of 1,3-butadiene with hydrogen cyanide to make 3-pentenenitrile is recycled. At least a portion of the recycled catalyst is purified by an extraction process, which separates catalyst degradation products and reaction byproducts, such as mononitriles having 9 carbon atoms, from the catalyst.

    Abstract translation: 己腈通过3-戊烯腈与氰化氢反应制得。 3-戊烯腈是通过使1,3-丁二烯与氰化氢反应制得的。 将1,3-丁二烯与氰化氢反应制成3-戊烯腈的催化剂被回收。 再循环催化剂的至少一部分通过萃取方法进行纯化,该方法从催化剂中分离出催化剂分解产物和反应副产物如具有9个碳原子的单腈。

    HYDROCYANATION OF 2-PENTENENITRILE
    9.
    发明申请
    HYDROCYANATION OF 2-PENTENENITRILE 审中-公开
    2-苯并噻唑的水解

    公开(公告)号:WO2008008927A3

    公开(公告)日:2008-12-18

    申请号:PCT/US2007073414

    申请日:2007-07-13

    Abstract: The invention provides a process for hydrocyanation, comprising: contacting 2-pentenenitrile with hydrogen cyanide at a temperature in the range of about 0°C to about 150°C in the presence of at least one Lewis acid promoter and a catalyst precursor composition, wherein the catalyst precursor composition comprises a zero-valent nickel and at least one bidentate phosphite ligand selected from a member of the group represented by Formula (I) and Formula (II), in which all like reference characters have the same meaning, except as further explicitly limited: wherein R1 and R5 are independently selected from the group consisting of C1 to C5 hydrocarbyl; and R2, R3, R4, R6, R7 and R8 are independently selected from the group consisting of H and C1 to C4 hydrocarbyl.

    Abstract translation: 本发明提供一种氢氰化方法,包括:在至少一种路易斯酸促进剂和催化剂前体组合物的存在下,在约0℃至约150℃的温度范围内使2-戊烯与氰化氢接触,其中 催化剂前体组合物包含零价镍和至少一种选自由式(I)和式(II)表示的基团的成员的二齿亚磷酸酯配体,其中所有相似的附图标记具有相同的含义,除了进一步 明确限制:其中R1和R5独立地选自C1-C5烃基; 并且R 2,R 3,R 4,R 6,R 7和R 8独立地选自H和C 1至C 4烃基。

    HYDROCYANATION PROCESS WITH REDUCED YIELD LOSSES
    10.
    发明申请
    HYDROCYANATION PROCESS WITH REDUCED YIELD LOSSES 审中-公开
    具有减少损失的油气化过程

    公开(公告)号:WO2008008926A3

    公开(公告)日:2008-12-04

    申请号:PCT/US2007073413

    申请日:2007-07-13

    CPC classification number: C07C253/10 C07C255/04

    Abstract: The invention provides a hydrocyanation process for the production of adiponitrile and other dinitriles having six carbon atoms, the process comprising: a) forming a reaction mixture in the presence of at least one Lewis acid, said reaction mixture comprising ethylenically unsaturated nitrites having five carbon atoms, hydrogen cyanide, and a catalyst precursor composition, by continuously feeding ethylenically unsaturated nitrites, hydrogen cyanide, and a catalyst precursor composition; b) controlling X and Z, wherein X is the overall feed molar ratio of 2-pentenenitriles to all unsaturated nitrites and Z is the overall feed molar ratio of hydrogen cyanide to all unsaturated nitrites, by selecting a value for X in the range from about 0.001 to about 0.5, and a value for Z in the range from about 0.5/1 to about 0.99/1, such that the value of quotient Q, Formula (I), wherein Q is in the range from about 0.2 to about 10, wherein 3PN is 3- pentenenitriles and 4PN is 4-pentenenitrile; and c) withdrawing a reaction product mixture comprising adiponitrile; wherein the ratio of the concentration of 2-pentenenitriles to the concentration of 3-pentenenitriles in the reaction mixture is from about 0.2/1 to about 10/1; wherein the catalyst precursor composition comprises a zero-valent nickel and at least one multidentate phosphorus-containing ligand; wherein the multidentate phosphorus-containing ligand is selected from the group consisting of a phosphite, a phosphonite, a phosphinite, a phosphine, and a mixed phosphorus-containing ligand or a combination of such members; and wherein the multidentate phosphorus-containing ligand gives acceptable results according to at least one protocol of the 2- Pentenenitrile Hydrocyanation Test Method.

    Abstract translation: 本发明提供用于生产具有六个碳原子的己二腈和其它二腈的氢氰化方法,该方法包括:a)在至少一种路易斯酸存在下形成反应混合物,所述反应混合物包含具有五个碳原子的烯属不饱和亚硝酸盐 ,氰化氢和催化剂前体组合物,通过连续进料烯属不饱和亚硝酸盐,氰化氢和催化剂前体组合物; b)控制X和Z,其中X是2-戊烯腈与所有不饱和亚硝酸盐的总进料摩尔比,Z是氰化氢与所有不饱和亚硝酸盐的总进料摩尔比,通过在约 0.001至约0.5,Z值在约0.5 / 1至约0.99 / 1的范围内,使得Q值在约0.2至约10的范围内的商Q,式(I) 其中3PN是3-戊烯腈,4PN是4-戊烯腈; 和c)取出包含己二腈的反应产物混合物; 其中所述2-戊烯腈的浓度与所述反应混合物中3-戊烯腈的浓度的比例为约0.2 / 1至约10/1; 其中所述催化剂前体组合物包含零价镍和至少一种多齿含磷配体; 其中所述多齿含磷配体选自亚磷酸盐,亚膦酸盐,次膦酸盐,膦和混合的含磷配体或这些成员的组合; 并且其中所述多齿含磷配体根据2-戊烯腈氢氰化测试方法的至少一个方案得到可接受的结果。

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