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A more detailed description of the processes can be seen in the drawing wherein the following procedure relative tozirconium oxychloride is illustrated. This invention for the preparation of zirconium oxychloride free from phosphorus is shown in the drawing wherein the sole FIGURE in the case sets forth a flow sheet and involves the following steps: (a) Dissolution of zirconium tetrachloride in water, recycled mother liquor and dissolved recycled zirconium oxychloride to form a solution having a temperature about 75° C, not greater than 1.1 M in zirconium and having a total acid no higher than 6.0 N. (b) Filtering the solution to remove any insoluble material and cooling to form pure zirconium oxychloride crystals and a mother liquor no higher in total acid than 5.75 N. (c) Separation of the crystal product from the mother liquor after cooling and not later than about 24 hours after the mixture was prepared. (d) Washing the crystals with 5.5 N hydrochloric acid. (e) Recycling a portion (usually 40%) of the mother liquor to be used in the preparation of a new batch of crystals as soon as it is separated from the crystals. (f) Evaporation of the remaining mother liquor to form crude zirconium oxychloride crystals. (g) Dissolution of these crude zirconium oxychloride crystals in cold water followed by immediate filtration to remove insoluble zirconium phosphate. (h) Recycling the clear solution of crude zirconium oxychloride from step (g) to step(a) In accordance with the above procedure, tests were run on various batches of material having various concentrations and normalities. Tables I and II summarize the results of two typical experiments showing the effect of total acid on phosphorus removal. The first experiment included batch tests at various acidities and two levels of phosphorus. The second experiment was a recycle test where a portion of the mother liquor was recycled each day in the preparation of a new batch of crystals. The effect of total acid is apparent in the P/Zr analysis of the product crystals. This criticality is particularly evident in Table II where it can be seen that a total acidity of the mother liquor at 5.65 N (Example 4) had good results, whereas Example 13 having a total acidity of 5.75 N, most of the phosphorus appears to have been precipitated out of solution. As this invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, the present embodiment is, therefore, illustrative and not restrictive, since the scope of the invention is defined by the appended claims rather than by the description preceding them, and all changes that fall within the mete and bounds of the claims or that form their functional as well as conjointly cooperative equivalent are, therefore, intended to be embraced by those claims. As, for instance, the same process illustrated by the production of zirconium oxychloride can be used for purification of hafnil,lIll oxychloride. |
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3楼2014-02-18 20:21:57
RXMCDM
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hancr: 金币+15, 翻译EPI+1, ★★★★★最佳答案 2014-02-18 20:21:21
hancr: 金币+15, 翻译EPI+1, ★★★★★最佳答案 2014-02-18 20:21:21
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A more detailed description of the processes can be seen in the drawing wherein the following procedure relative tozirconium oxychloride is illustrated. This invention for the preparation of zirconium oxychloride free from phosphorus is shown in the drawing wherein the sole FIGURE in the case sets forth a flow sheet and involves the following steps: (a) Dissolution of zirconium tetrachloride in water, recycled mother liquor and dissolved recycled zirconium oxychloride to form a solution having a temperature about 75° C, not greater than 1.1 M in zirconium and having a total acid no higher than 6.0 N. (b) Filtering the solution to remove any insoluble material and cooling to form pure zirconium oxychloride crystals and a mother liquor no higher in total acid than 5.75 N. (c) Separation of the crystal product from the mother liquor after cooling and not later than about 24 hours after the mixture was prepared. (d) Washing the crystals with 5.5 N hydrochloric acid. (e) Recycling a portion (usually 40%) of the mother liquor to be used in the preparation of a new batch of crystals as soon as it is separated from the crystals. (f) Evaporation of the remaining mother liquor to form crude zirconium oxychloride crystals. (g) Dissolution of these crude zirconium oxychloride crystals in cold water followed by immediate filtration to remove insoluble zirconium phosphate. (h) Recycling the clear solution of crude zirconium oxychloride from step (g) to step(a) In accordance with the above procedure, tests were run on various batches of material having various concentrations and normalities. 图中示出了更详细的过程描述，下面说明有关氧氯化锆的过程。 本发明的氧氯化锆制备不受磷的影响，示于附图中，其中唯一的附图示出了流程表并包括以下步骤： （a）四氯化锆溶解于水，循环母液和回收溶解的氧氯化锆制成溶液，温度约75℃ ，锆不大于1.1 M和总酸值不大于6.0 N。 （ b）过滤该溶液以除去任何不溶性物质，并冷却，形成纯的氧氯化锆晶体，母液总酸值不高于5.75 N。 （c）从母液中分离结晶产物,制备的混合物冷却后但不超过(约)24小时。 （d）5.5当量的盐酸洗涤晶体。 （e）母液与晶体分离后，循环使用母液的一部分（通常是40％）用于新晶体制备。 （f）剩余的母液蒸发以形成粗氧氯化锆晶体。 （g）用冷水溶解这些粗制氧氯化锆结晶，然后立即过滤除去不溶性锆磷酸盐。 （h）回收粗制氯氧化锆的上清液，从步骤（g）回到步骤（a ） 按照上述过程，测试不同批次材料的不同浓度和当量浓度。 |
2楼2014-02-18 15:54:17
RXMCDM
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4楼2014-02-18 22:07:42
