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Production of certain hitherto undescribed acid esters of orthophosphoric acid and their salts

机译:某些迄今未描述的正磷酸酸酯及其盐的生产

摘要

The invention comprises p-tert. octyl-phenyl dihydrogen phosphate in the state of a solid crystalline compound, and p-tert. octyl-cresyl dihydrogen phosphates. It also includes a process for the production of p-tert. octylphenyl dihydrogen phosphate and p-tert. octylcresyl dihydrogen phosphates which comprises gradually adding a quantity of water, which after allowing for losses by evaporation and entrainment, amounts to 2 mols. of water to 1 mol. of p-tert. octyl-phenoxy phosphoryl dichloride or p-tert. octyl cresoxy phosphoryl dichloride heated to a reaction temperature, removing the hydrogen chloride formed and keeping the reaction mixture fluid until the reaction is completed by control of the reaction temperature, the rate of addition of water being such that no aqueous layer accumulates. An indifferent gas, e.g. nitrogen, air or carbon dioxide may be passed through the mixture to assist removal of hydrogen chloride. Initially, the reaction temperature may be 85 DEG to 90 DEG C., and towards the end may be raised to 120 DEG to 140 DEG C. The acid phosphate may be converted into a salt by mixing it with an aqueous solution of a base in just sufficient water to enable the resulting salt to be obtained in the form of a paste. Examples of the preparation of the two products are given. The products are useful as frothing and coating agents (see Groups II, III and IV (c)). p-tert. Octyl-cresoxy-phosphoryl dichloride is obtained by heating p-tert. octyl-cresol with an excess of phosphorus oxychloride in the presence of metallic iron.ALSO:Solutions of low concentration of the salts of p-tert octyl-phenyl dihydrogen phosphate and p-tert. octyl-cresyl dihydrogen phosphates are used for coating artificial fibres for spinning to import anti-slipping properties. The preparation of such phosphates and their salts is described (see Group IV(b)).ALSO:p-tert. Octyl-phenyl dihydrogen phosphate and p-tert octyl-cresyl dihydrogen phosphates in small concentrations act as anti-corrosives for ferrous and non-ferrous metals, especially when associated with the presence of an oil. Aqueous solutions of salts of such esters also confer non-slipping properties when a thin film is allowed to evaporate on a smooth surface for example metals, glass, tiles, smooth flooring materials and other smooth materials. The preparation of these compounds is described (see Group IV (b)).ALSO:p-tert. Octyl-phenyl dihydrogen phosphate and p-tert octyl-cresyl dihydrogen phosphates and their salts are suitable for use in froth flotation operations as collecting agents for mineral ores. They float fluorspor, barytes, calcite, chromite, and ilmenite but not quartz. They retain foaming properties between pH values of about 1.0 to 8.0. The preparation of these compounds is described, (see Group IV (b)).
机译:本发明包括p-叔胺。辛基-苯基磷酸二氢酯为固态结晶化合物和对-叔丁基。辛基-甲苯基二氢磷酸酯。它还包括生产p-叔叔的过程。磷酸辛基苯基二氢酯和对叔丁基。辛基甲苯基二氢磷酸酯,其包括逐渐添加一定量的水,该水在通过蒸发和夹带而损失后总计为2摩尔。水至1摩尔。 p-tert。辛基-苯氧基磷酰二氯或对-叔丁基。通过控制反应温度,将辛基甲氧基甲氧基磷酰二氯加热至反应温度,除去形成的氯化氢并使反应混合物保持流体直至反应完成,水的添加速率使得没有水层积聚。无味气体,例如可以使氮气,空气或二氧化碳通过该混合物,以帮助除去氯化氢。最初,反应温度可以为85℃至90℃,并且最后可以升高至120℃至140℃。可以通过将其与碱的水溶液混合,将酸性磷酸酯转化为盐。仅仅足够的水以使得能够以糊状形式获得所得到的盐。给出了两种产品的制备实例。该产品可用作起泡剂和涂层剂(参见II,III和IV(c)组)。 p-tert。辛基-甲氧基-磷酰二氯通过加热对-叔丁基获得。在金属铁存在下,用过量的三氯氧化磷制备辛基甲酚。ALSO:对-叔辛基-苯基磷酸二氢酯和对-叔丁基盐的低浓度溶液。辛基-甲苯基二氢磷酸酯用于涂覆人造纤维以纺丝,以增强防滑性。描述了这种磷酸盐及其盐的制备(参见IV(b)组)。少量的辛基-苯基二氢磷酸酯和对叔辛基-甲苯基二氢磷酸酯可作为黑色金属和有色金属的防腐剂,尤其是与油的存在有关时。当允许薄膜在光滑的表面(例如金属,玻璃,瓷砖,光滑的地板材料和其他光滑的材料)上蒸发时,此类酯的盐的水溶液也赋予防滑性能。描述了这些化合物的制备(参见第IV(b)组)。ALSO:p-tert。辛基苯基磷酸二氢酯和对叔辛基甲苯基磷酸二氢酯及其盐适合作为矿物矿石的收集剂用于泡沫浮选操作中。它们会漂浮萤石,重晶石,方解石,铬铁矿和钛铁矿,但不会漂浮石英。它们在约1.0至8.0的pH值之间保持起泡性能。描述了这些化合物的制备(参见第IV(b)组)。

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