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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樓2014-02-18 20:21:57
RXMCDM
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【答案】應(yīng)助回帖
★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★ ★
hancr: 金幣+15, 翻譯EPI+1, ★★★★★最佳答案 2014-02-18 20:21:21
hancr: 金幣+15, 翻譯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. 圖中示出了更詳細的過程描述，下面說明有關(guān)氧氯化鋯的過程。 本發(fā)明的氧氯化鋯制備不受磷的影響，示于附圖中，其中唯一的附圖示出了流程表并包括以下步驟： （a）四氯化鋯溶解于水，循環(huán)母液和回收溶解的氧氯化鋯制成溶液，溫度約75℃ ，鋯不大于1.1 M和總酸值不大于6.0 N。 （ b）過濾該溶液以除去任何不溶性物質(zhì)，并冷卻，形成純的氧氯化鋯晶體，母液總酸值不高于5.75 N。 （c）從母液中分離結(jié)晶產(chǎn)物,制備的混合物冷卻后但不超過(約)24小時。 （d）5.5當(dāng)量的鹽酸洗滌晶體。 （e）母液與晶體分離后，循環(huán)使用母液的一部分（通常是40％）用于新晶體制備。 （f）剩余的母液蒸發(fā)以形成粗氧氯化鋯晶體。 （g）用冷水溶解這些粗制氧氯化鋯結(jié)晶，然后立即過濾除去不溶性鋯磷酸鹽。 （h）回收粗制氯氧化鋯的上清液，從步驟（g）回到步驟（a ） 按照上述過程，測試不同批次材料的不同濃度和當(dāng)量濃度。 |
2樓2014-02-18 15:54:17
RXMCDM
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- 性別: GG
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- 管轄: 論文翻譯
4樓2014-02-18 22:07:42
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