201141789 六、發明說明： 【發明所屬之技術領域】 本發明係關於-種製備六水氯化㈣方法。 【先前技術】 板的材:Γ在液晶玻璃基板中，作為玻璃基 的六水：：場需求量逐年增長，傳統技術製備 乾硬kg由於游離水分含量不穩定，極易發生結塊、 深入研ί成：用二大的困難。發明人對結塊機制進行了 水，九’/、水I化銷的結塊是由於其含有量的游離 觸的ί上六水氯化_溶解度極大，所以在晶體和晶體接 父界處造成溶解.成長過程，在成絲程中又把游離水 出造成更大範_溶解·成長直到大範圍結塊。 【發明内容】 題。本發明主要目的在於解決六水氣化銷材料的結塊問 發明人在研究結塊機制的基礎上改良了傳統製備技 好日透過二次烘乾晶體表面過供固化技術，使得六水氯化 ^曰，曰體的表面失水’亦即使晶體表面部分並非為六個結晶 進而改善了溶解-成長所造成的結塊問題。 -種製備六水氯化鳃的方法，包括以下步驟： (1) 將SrC03加水製成液體，加入鹽酸溶解，得到溶液； (2) 在步驟⑴所得溶液中加入過氧化氮，將鐵⑽⑯ 201141789 化； (3) 將步驟（2)所得溶液加熱至沸騰後，用 Sr(OHV8H2〇調整該溶液至ρΗ=8·9 ; (4) 將步驟(3)所得溶液壓濾分離，將所得澄清液蒸發濃 縮至波美度48-50，此蒸發操作一般在蒸發罐内進 行；再將所得澄清液冷卻結晶，此結晶操作一般在 冷卻結晶罐中進行； 其中’步驟(4)中的兩次壓濾均可透過壓濾機進行。 (5) 將步驟(4)所得結晶壓濾分離’將壓濾分離所得固體 結晶烘乾’控制物料游離水分含量（重量百分比） £2%，然後再利用熱氣流對結晶進行洪乾操作，此 烘乾操作可以在氣流烘乾裝置中進行，控制結晶游 離水分含量（重量百分比）$〇.2%，冷卻後即得 SrCl2.6H20。 較佳地，該步驟（5)還可以包括將壓滤分離所得母液導 回至製備的SrCCh溶液的步驟，此時步驟（丨）為在SrC〇3中 加入此母液製備液體。 較佳地’該步驟(5)中第一次烘乾可利用振動流化床進 行。 較佳地’該步驟(5)中熱氣流烘乾操作中熱氣流的溫度 為 180-230°C。 本發明的主要化學反應為：201141789 VI. DESCRIPTION OF THE INVENTION: TECHNICAL FIELD OF THE INVENTION The present invention relates to a method for preparing hexahydrate chlorination (IV). [Prior Art] The material of the board: Γ in the liquid crystal glass substrate, as the glass-based Liushui: The field demand is increasing year by year. The conventional technology for preparing dry hard kg is prone to agglomeration due to unstable free moisture content. ί成: Use two major difficulties. The inventor carried out water on the agglomeration mechanism, and the agglomeration of the water is due to its content of free contact. The chlorination of the hexahydrate _ solute is extremely large, so it is caused at the junction of the crystal and the crystal. Dissolution. During the growth process, the free water is released into a larger range in the silking process. Dissolve and grow until a large extent of agglomeration. SUMMARY OF THE INVENTION The main object of the present invention is to solve the agglomeration of the Liushui gasification pin material. The inventor has improved the traditional preparation technique on the basis of the agglomeration mechanism to chlorinate the hexahydrate through the secondary drying crystal surface over-hardening technology. ^曰, the surface of the carcass loses water' even if the surface portion of the crystal is not six crystals, which improves the caking problem caused by dissolution-growth. - a method for preparing cerium chloride hexahydrate, comprising the following steps: (1) adding SrC03 to water to form a liquid, adding hydrochloric acid to dissolve to obtain a solution; (2) adding nitrogen peroxide to the solution obtained in the step (1), and adding iron (10) 16 201141789 (3) After heating the solution obtained in the step (2) to boiling, the solution is adjusted to ρΗ=8·9 with Sr(OHV8H2〇; (4) the solution obtained in the step (3) is separated by pressure filtration, and the resulting clear liquid is obtained. Evaporation and concentration to Baume 48-50, the evaporation operation is generally carried out in an evaporation tank; the resulting clear liquid is cooled and crystallized, and the crystallization operation is generally carried out in a cooling crystallization tank; wherein the two pressures in the step (4) Filtration can be carried out through a filter press. (5) Separating the crystallization obtained in step (4) by pressure filtration 'drying the solid crystal obtained by pressure filtration to separate 'control the free moisture content (% by weight) of the material by £2%, and then using the hot gas The stream is subjected to a lyophilization operation, and the drying operation can be carried out in a gas flow drying device to control the crystallization free moisture content (% by weight) of 〇.2%, and after cooling, SrCl2.6H20 is obtained. Preferably, this step (5) may also include pressure filtration The step of separating the obtained mother liquid back to the prepared SrCCh solution, at this time, the step (丨) is to add the mother liquid to prepare the liquid in SrC〇3. Preferably, the first drying in the step (5) can utilize the vibrating flow. Preferably, the temperature of the hot gas stream in the hot gas drying operation in the step (5) is 180-230 ° C. The main chemical reaction of the present invention is:
SrC03+2HCl — SrCl2+H20+C02T MgCl2+Sr(0H)2+H20 —Mg(OH)2i+SrCl2 201141789SrC03+2HCl — SrCl2+H20+C02T MgCl2+Sr(0H)2+H20 —Mg(OH)2i+SrCl2 201141789
Fe2++H202 -> Fe3+ -> Fe(OH)3| 利用本發明的方法製備的六水氯化锶產品外觀上為疏 鬆晶體，游離水含量穩定，小於0.2%，大幅改善結塊問題； 並且用本方法製備的六水氯化勰產品雜質成分少，解決了 液晶玻璃基板中所用六水氯化锶材料結塊問題，可滿足下 . 游產業輸送、配料、混合程序的要求。 ψ % 【實施方式】 實施例1 在Vg 10m3搪玻反應罐内加入2 m3母液，加入3公°頓 工業級碳酸锶，攪拌下加入工業鹽酸溶解； 然後加入25公升濃度27.5%工業級過氧化氫，進行氧 化反應； 將氧化後的溶液加熱煮彿，用Sr(0H)2‘8H20調節 pH=8 ； 將調節後的溶液用壓濾機過濾，澄清液移至蒸發罐 内，蒸發濃縮至48波美度後，澄清液移至冷卻結晶罐内， 冷卻結晶； Γ 將結晶操作後的結晶吸濾分離，將上述吸濾後固體結 ; 晶用振動流化床進行一次烘乾，測得結晶游離水分為1.9% 後，再將結晶用氣流乾燥裝置進行二次烘乾，其中熱氣流 溫度為180°C，測得結晶游離水分為0.16%，停止烘乾，待 結晶冷卻後，可得SrCl2‘6H20樣品1#。 201141789 實施例2 在Vg 1 Om3搪玻反應罐内加入2 m3母液，加入3公π頓 工業級碳酸勰，攪拌下加入工業鹽酸溶解； 在所得溶液中加入25公升27.5%工業級過氧化氫，進 行氧化反應； 加熱煮沸，用Sr(0H)2’8H20調節ρΗ=9 ; 將調節後的溶液用壓濾機過濾，澄清液移至蒸發罐 内，蒸發濃縮至50波美度後，所得澄清液移至冷卻結晶罐 内，冷卻結晶； 將結晶彳呆作後的結晶吸滤·分離’將上述吸滤·分離後固 體結晶用振動流化床進行一次烘乾，測得結晶游離水分為 1.7%，之後再將結晶用氣流乾燥裝置進行二次烘乾，其中 熱氣流溫度為230°C，測得結晶游離水分為0.10%，停止烘 乾，待結晶冷卻後，獲得SrCl2’6H20樣品2#。 以上實施例所得產品的參數如下表：Fe2++H202 -> Fe3+ -> Fe(OH)3| The ruthenium chloride hexahydrate product prepared by the method of the invention has loose crystal appearance, stable free water content, less than 0.2%, and greatly improves the caking problem. Moreover, the cerium chloride hexahydrate product prepared by the method has less impurity components, and solves the problem of agglomeration of the cerium chloride hexahydrate material used in the liquid crystal glass substrate, and can meet the requirements of the transportation, compounding and mixing procedures of the tourism industry. ψ % [Embodiment] Example 1 2 m3 mother liquor was added to a Vg 10m3 glass-reactor, 3 industrial grade cesium carbonate was added, and industrial hydrochloric acid was dissolved under stirring; then 25 liters of concentration of 27.5% industrial grade peroxidation was added. Hydrogen, carry out oxidation reaction; heat the oxidized solution to boil, adjust pH=8 with Sr(0H)2'8H20; filter the adjusted solution with a filter press, move the clear liquid to the evaporation tank, and concentrate by evaporation to After 48 Baume, the clear liquid is moved to the cooling crystallization tank to cool the crystal; Γ The crystal after the crystallization operation is separated by suction filtration, and the solid precipitate after suction filtration is used; the crystal is dried once by a vibrating fluidized bed, and measured. After the crystal free moisture is 1.9%, the crystallization is secondarily dried by a gas flow drying device, wherein the hot gas flow temperature is 180 ° C, and the crystal free moisture is measured to be 0.16%, the drying is stopped, and after the crystal is cooled, the crystal is obtained. SrCl2'6H20 sample 1#. 201141789 Example 2 2 m3 mother liquor was added to a Vg 1 Om3 glass reactor, 3 metric tons of industrial grade cesium carbonate was added, and industrial hydrochloric acid was added with stirring; 25 liters of 27.5% industrial grade hydrogen peroxide was added to the obtained solution. The oxidation reaction was carried out; the mixture was heated and boiled, and ρΗ=9 was adjusted with Sr(0H)2'8H20; the adjusted solution was filtered with a filter press, and the clear liquid was transferred to an evaporation can, and concentrated to 50 Baume after evaporation to obtain clarification. The liquid is transferred to a cooling crystallization tank to cool the crystal; the crystallization of the crystallization remains after suction filtration/separation. The solid crystallization of the above-mentioned suction filtration and separation is once dried by a vibrating fluidized bed, and the crystal free moisture is measured to be 1.7. %, and then the crystallization is secondarily dried by a gas flow drying device, wherein the temperature of the hot gas stream is 230 ° C, and the measured free moisture of the crystal is 0.10%, the drying is stopped, and after cooling by the crystal, the sample of SrCl 2 '6H20 is obtained 2# . The parameters of the products obtained in the above examples are as follows:
SrCl2-6H20 1# SrCl2*6H20 2# SrCl2-6H20 (重量百分比含量） 99.84 99.90 Fe PPm <5 <5 Mg PPm <1 <1 游離水 (重量百分比含量） 0.16 0.10 外觀 疏鬆晶體 疏鬆晶體 201141789 【圖式簡單說明】 第1圖為本發明的主要技術流程圖。 【主要元件符號說明】SrCl2-6H20 1# SrCl2*6H20 2# SrCl2-6H20 (% by weight) 99.84 99.90 Fe PPm <5 <5 Mg PPm <1 <1 free water (% by weight) 0.16 0.10 Appearance loose crystal loose crystal 201141789 [Simple description of the drawings] Fig. 1 is a main technical flow chart of the present invention. [Main component symbol description]