Polyphosphazene process
    2.
    发明授权
    Polyphosphazene process 失效
    聚磷腈工艺

    公开(公告)号:US4568779A

    公开(公告)日:1986-02-04

    申请号:US601506

    申请日:1984-04-18

    摘要: A process for making an alkali metal alkoxide (e.g. sodium alkoxide) of a halogen-substituted alcohol (e.g. fluorine-substituted alcohols) by dispersing an alkali metal (e.g. sodium) in a cycloalkane (e.g. cyclohexane) and adding the resultant dispersion to an ether (e.g. THF) solution of a halogen-substituted alcohol. The resultant alkali metal haloalkoxide solution can be reacted with a phosphonitrilic chloride polymer to introduce haloalkoxide substituents.

    摘要翻译: 通过将碱金属(例如钠)分散在环烷烃(例如环己烷)中制备卤素取代的醇(例如氟取代的醇)的碱金属醇盐(例如烷氧基化钠)的方法,并将所得分散体加入到醚 (例如THF)溶液。 得到的碱金属卤代醇盐溶液可与磷酰氯化聚合物反应以引入卤代醇盐取代基。

    Preventing undesired odor in and/or purifying alkanediols
    3.
    发明授权
    Preventing undesired odor in and/or purifying alkanediols 失效
    预防烷基二醇中和/或纯化不良气味

    公开(公告)号:US06528665B1

    公开(公告)日:2003-03-04

    申请号:US10116482

    申请日:2002-04-03

    IPC分类号: C07D30132

    摘要: Epoxyalkanes are subjected to at least one of the following washing operations: (1) washing with aqueous inorganic base, and then with aqueous borohydride, or vice versa; or (2) washing with an aqueous solution of both inorganic base and borohydride. Undesirable odor is reduced or eliminated from alkanediol(s), if produced from the treated epoxyalkane(s) by hydrolysis. Use of such washing procedures in the production of alkanediols is also described.

    摘要翻译: 对环氧烷烃进行以下洗涤操作中的至少一种:(1)用无机碱水溶液洗涤,然后用硼氢化钠洗涤,反之亦然; 或(2)用无机碱和硼氢化钠的水溶液洗涤。 如果通过水解由经处理的环氧烷烃生产,则从链烷二醇中减少或消除不希望的气味。 还描述了在制备链烷二醇中使用这种洗涤方法。

    Epoxidation of olefins
    4.
    发明授权
    Epoxidation of olefins 失效
    烯烃环氧化

    公开(公告)号:US06525208B1

    公开(公告)日:2003-02-25

    申请号:US10116508

    申请日:2002-04-03

    IPC分类号: C07D30112

    CPC分类号: C07D301/12

    摘要: Mixed together are (i) hydrogen peroxide; (ii) 1-alkene; (iii) quaternary ammonium salt wherein at least one of the substituents contains at least six carbon atoms; (iv) boric acid, or both a 1,2-diol and boric acid; and (v) a preformed catalyst solution formed from hydrogen peroxide, at least one aqueous inorganic acid, and at least one tungstate salt, while water is continuously removed, such that a 1,2-epoxide is formed. A new method for purifying 1,2-epoxyalkanes is also described.

    摘要翻译: 混合在一起是(i)过氧化氢; (ii)1-烯烃; (iii)季铵盐,其中至少一个取代基含有至少6个碳原子; (iv)硼酸,或1,2-二醇和硼酸; 和(v)由过氧化氢,至少一种含水无机酸和至少一种钨酸盐形成的预成型催化剂溶液,同时连续除去水,从而形成1,2-环氧化物。 还描述了用于纯化1,2-环氧烷烃的新方法。

    Inhibiting ferrous metal corrosion by aqueous ammoniate solutions
    5.
    发明授权
    Inhibiting ferrous metal corrosion by aqueous ammoniate solutions 失效
    用氨水溶液抑制黑色金属腐蚀

    公开(公告)号:US5871667A

    公开(公告)日:1999-02-16

    申请号:US786536

    申请日:1997-01-21

    CPC分类号: C07F9/224 C23F11/06

    摘要: Aqueous ammoniate solutions made during the manufacture of N-hydrocarbyl thiophosphoric triamides, consisting essentially of aqueous solutions of ammonium chloride and ammonia containing a water-soluble impurity normally tending to engender corrosion of ferrous metal are rendered corrosion-resistant by dissolving therein a small corrosion-inhibiting amount (e.g., up to about 5000 ppm (wt/wt) of a water-soluble salt or oxide of zinc, aluminum, arsenic, antimony or bismuth.

    摘要翻译: 在制造N-烃基硫代磷酸三酰胺期间制备的氨水溶液,其基本上由氯化铵的水溶液和含有通常倾向于引起黑色金属腐蚀的水溶性杂质的氨制成耐腐蚀性, 抑制量(例如,高达约5000ppm(wt / wt)的锌,铝,砷,锑或铋的水溶性盐或氧化物。

    Preparation of N-hydrocarbylthiophosphoric triamides
    6.
    发明授权
    Preparation of N-hydrocarbylthiophosphoric triamides 失效
    N-烃基硫代磷酸三酰胺的制备

    公开(公告)号:US5770771A

    公开(公告)日:1998-06-23

    申请号:US786396

    申请日:1997-01-21

    摘要: Continuously fed to and mixed in a first reactor are (i) a preformed mixture of primary hydrocarbyl monoamine, tertiary amine and liquid inert organic solvent, and (ii) thiophosphoryl chloride while removing heat of reaction to maintain the reaction temperature in the range of about -20.degree. C. to about +50.degree. C. A reaction mixture containing N-hydrocarbylaminothiophosphoryl dichloride is formed. Ammonia and an effluent stream from the first reactor are continuously fed to and mixed in a second reactor in proportions of at least about 16 moles, of ammonia per mole of N-hydrocarbylaminothiophosphoryl dichloride that produce a reaction mixture containing N-hydrocarbylthiophosphoric triamide, and that keep in solution ammonium chloride co-product formed in the reaction. Heat of reaction is removed so that the temperature is high enough to keep ammonium chloride-ammonia complex from forming a solid phase in this reaction mixture, but low enough to avoid significant reduction in yield of N-hydrocarbylthiophosphoric triamide being formed. Effluent is withdrawn from the second reactor so as to maintain a substantially constant volume of reaction mixture in the second reactor. The process eliminates a difficult filtration of the co-product ammonium chloride formed in the second reaction. Also, it possible to accomplish this in a continuous process, with improved efficiency in large scale production of the N-hydrocarbylthiophosphoric triamides. Moreover, the ammonium chloride can be readily converted in the process to an industrially useful liquid co-product mixture.

    摘要翻译: 连续进料并混合在第一反应器中的是(i)主要烃基单胺,叔胺和液体惰性有机溶剂的预制混合物,和(ii)硫代磷酰氯,同时除去反应热,将反应温度保持在约 -20℃至约+ 50℃。形成含有N-烃基氨基硫代磷酰基二氯化物的反应混合物。 将氨和来自第一反应器的流出物流连续地进料至第二反应器中,其比例为至少约16摩尔,每摩尔N-烃基氨基硫代磷酰二氯的氨,其产生含有N-烃基硫代磷酰三酰胺的反应混合物,并且 保持反应中形成的溶液中氯化铵共同产物。 去除反应热,使得温度足够高以使氯化铵 - 氨络合物在该反应混合物中形成固相,但足够低以避免形成的N-烃基硫代磷酰三酰胺的产率显着降低。 将废水从第二反应器中排出,以便在第二反应器中维持反应混合物体积基本恒定。 该方法消除了在第二反应中形成的副产物氯化铵的难以过滤。 此外,可以在连续的方法中实现这一点,提高N-烃基硫代磷酸三酰胺的大规模生产的效率。 此外,氯化铵可以在工艺中容易地转化成工业上有用的液体共产物混合物。

    Cyclic phosphonitrilic halide process
    7.
    发明授权
    Cyclic phosphonitrilic halide process 失效
    环状膦酰氯化物工艺

    公开(公告)号:US4656018A

    公开(公告)日:1987-04-07

    申请号:US798910

    申请日:1985-11-18

    IPC分类号: C01B21/098 C01B25/10

    CPC分类号: C01B21/098 C01B21/0986

    摘要: Cyclic phosphonitrilic halide trimer is made in high yield and at a rapid rate by adding NH.sub.3 or ammonium halide to a pyridine-hydrogen halide complex and adding phosphorus pentahalide and a solvent for the trimer (e.g. monochlorobenzene) and heating the mixture to above 90.degree. C. to form trimer which dissolves in the solvent and then separating the trimer-solvent phase from the residue phase of pyridine-hydrogen halide complex and recovering trimer from the solvent phase and recycling the pyridine-hydrogen halide phase to a subsequent procedure conducted in the same manner. The process can also be adapted to produce linear species in high yield also.

    摘要翻译: 通过向吡啶 - 卤化氢络合物中加入NH 3或卤化铵并加入五氯化磷和三聚物(例如一氯苯)的溶剂并将混合物加热到90℃以上,以高产率和快速的速率制备环状膦酰氯化物三聚体 形成溶解在溶剂中的三聚体,然后将三聚体 - 溶剂相与吡啶 - 卤化氢络合物的残留相分离并从溶剂相中回收三聚体并将吡啶 - 卤化氢相再循环到随后的相同步骤中 方式。 该方法还可以适应于以高产率生产线性物种。

    Recovery of N-hydrocarbylthiophosphoric triamides and
N-hydrocarbylphosphoric triamides from reaction mixtures
    8.
    发明授权
    Recovery of N-hydrocarbylthiophosphoric triamides and N-hydrocarbylphosphoric triamides from reaction mixtures 失效
    从反应混合物中回收N-烃基硫代磷酸三酰胺和N-烃基磷酸三酰胺

    公开(公告)号:US5955630A

    公开(公告)日:1999-09-21

    申请号:US786535

    申请日:1997-01-21

    IPC分类号: C07F9/02 C07F9/22

    CPC分类号: C07F9/224 C07F9/025

    摘要: N-hydrocarbylthiophosphoric triamide is separated or recovered from a liquid mixture comprising N-hydrocarbylthiophosphoric triamide, inert organic solvent, and optionally but preferably, tertiary amine, by continuously introducing a stream of the liquid mixture into a wiped film evaporator operating at a temperature in the range of about 60 to about 140.degree. C., and at a pressure that avoids solids formation on the heating surface of the wiped film evaporator, and continuously collecting the resultant N-hydrocarbylthiophosphoric triamide product.

    摘要翻译: 通过将液体混合物流连续地引入到在该温度下操作的擦拭膜蒸发器中,从包含N-烃基硫代磷酸三酰胺,惰性有机溶剂和任选但优选叔胺的液体混合物中分离或回收N-烃基硫代磷酰三胺 范围为约60至约140℃,并且具有避免在刮膜蒸发器的加热表面上形成固体的压力,并连续收集所得的N-烃基硫代磷酰三胺产物。

    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or
N-hydrocarbylphosphoric triamides
    9.
    发明授权
    Preparation and recovery of N-hydrocarbylthiophosphoric triamides or N-hydrocarbylphosphoric triamides 失效
    N-烃基硫代磷酸三酰胺或N-烃基磷酸三酰胺的制备和回收

    公开(公告)号:US5883297A

    公开(公告)日:1999-03-16

    申请号:US58367

    申请日:1998-04-09

    摘要: A reaction mixture containing N-hydrocarbylthiophosphoric triamide or N-hydrocarbylphosphoric triamide ("Triamide") is formed by reacting ammonia with N-hydrocarbylaminothiophosphoryl dichloride or N-hydrocarbylaminophosphoryl dichloride in a liquid organic medium, in proportions of at least 16 moles of ammonia per mole of such dichloride and that keep in solution the ammonium chloride co-product formed in the reaction. The temperature of the reaction mixture is kept high enough to keep ammonium chloride-ammonia complex from forming a solid phase in the reaction mixture, but low enough to avoid significant reduction in Triamide yield. The reaction mixture is then caused/allowed to separate into an inorganic phase comprising ammonia, ammonium chloride and co-product thiophosphoric triamide or phosphoric triamide, and an organic phase comprising Triamide, liquid organic medium, dissolved ammonia and, usually, phosphorus impurities. These phases are separated from each other. The ammonia is removed from the organic phase to leave a concentrated solution of Triamide in residual liquid organic medium usually also containing phosphorus impurities. The Triamide is separated or recovered from this residual mixture by continuously introducing a stream of the liquid mixture into a wiped film evaporator operating at a temperature of about 60.degree.-140.degree. C., and at a pressure that avoids solids formation on the heating surface of the wiped film evaporator, and continuously collecting the Triamide product. Triamides are urease inhibitors for use with urea-based fertilizers.

    摘要翻译: 通过使氨与N-烃基氨基硫代磷酰基二氯化物或N-烃基氨基磷酰基二氯化物在液体有机介质中反应,按每摩尔至少16摩尔氨的比例形成含有N-烃基硫代磷酰三胺或N-烃基磷酸三酰胺(“三酰胺”)的反应混合物 的这种二氯化物,并保持溶液中形成的氯化铵副产物在反应中。 反应混合物的温度保持足够高以保持氯化铵 - 氨络合物在反应混合物中形成固相,但足够低以避免三酰胺产率的显着降低。 然后使反应混合物分离成包含氨,氯化铵和副产物硫代磷酸三酰胺或磷酸三酰胺的无机相,以及包含三酰胺,液体有机介质,溶解氨和通常为磷杂质的有机相。 这些阶段相互分离。 从有机相中除去氨,留下通常也含有磷杂质的残留液体有机介质中的三酰胺浓缩溶液。 通过将液体混合物流连续地引入到在约60-140℃的温度下操作的擦拭膜蒸发器中并且在避免在加热表面上形成固体的压力下将三酰胺分离或回收 的擦拭膜蒸发器,并连续收集三酰胺产物。 三酰胺是用于尿素肥料的尿素酶抑制剂。

    Separating ammonium chloride from N-hydrocarbylphosphoric triamide or
N-hydrocarbylthiophosphoric triamide
    10.
    发明授权
    Separating ammonium chloride from N-hydrocarbylphosphoric triamide or N-hydrocarbylthiophosphoric triamide 失效
    从N-烃基磷酸三酰胺或N-烃基硫代磷酸三酰胺中分离氯化铵

    公开(公告)号:US5872293A

    公开(公告)日:1999-02-16

    申请号:US785104

    申请日:1997-01-21

    CPC分类号: C01C1/164 C07F9/025 C07F9/224

    摘要: A substantially anhydrous mixture which comprises ammonium chloride, the triamide, and ammonia is formed either by adding ammonia to a mixture of the other components or by conducting, in the presence of the ammonia and an organic solvent, a reaction to form the triamide and ammonium chloride as co-products. In all cases the ammonia is present in a sufficient excess amount relative to the ammonium chloride to form a separate liquid phase in which the ammonium chloride solids dissolve. Such separate liquid phase is separated from the remainder of said mixture.

    摘要翻译: 包含氯化铵,三酰胺和氨的基本上无水的混合物通过向其它组分的混合物中加入氨或在氨和有机溶剂的存在下进行形成三酰胺和铵的反应形成 氯化物作为副产物。 在所有情况下,相对于氯化铵,氨以足够的过量存在,以形成其中氯化铵固体溶解的单独液相。 这种分离的液相与所述混合物的其余部分分离。