CN115259317A - 一种分离纯化聚合氯化钛优势水解产物的方法 - Google Patents
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Abstract
本发明提供了一种分离纯化聚合氯化钛优势水解产物的方法，包括以下步骤：（1）制备获得聚合氯化钛溶液；（2）向聚合氯化钛溶液中加入硫酸盐溶液进行沉淀，固液分离，液体即为聚合氯化钛优势水解产物的溶液；硫酸盐中硫酸根与聚合氯化钛中钛的摩尔比为1:1‑8:1。本发明相比通过分子量超滤的分离方法，易于操作，成本低，环境友好，易于获得富含优势水解形态的钛基盐混凝剂。
Description
技术领域
本发明属于污水处理技术领域，具体涉及一种分离纯化聚合氯化钛优势水解产物的方法。
背景技术
近年来，钛盐因其高效无毒受到广泛关注，钛盐混凝剂的研究已逐步从单体钛盐转向无机高分子类型以及各种复合类型，并且着重于聚合钛盐混凝剂的制备与应用。经钛盐混凝后的污泥煅烧可得到二氧化钛，且二氧化钛广泛应用于光催化、新能源电池、生物等行业。
但钛的水解形态分布及优势絮凝形态的鉴定分离仍然是当前研究的热点和难点。已有研究证明钛的多核羟基络合物的存在，并将聚合氯化钛中钛的水解产物分为Tia、Tib、Tic三类，Tia是由钛单体和钛的二聚体组成，Tib是由成千上百种钛的低聚物（Ti3-Ti8）和中聚物（Ti9-Ti16）组成，Tic则是由钛的高聚物（>Ti16）组成。目前聚合钛盐混凝过程中起主要作用的水解形态或某一聚合度的产物并没有更多的研究。现有技术中，分离聚合氯化钛优势水解形态的方法为采用超滤以分子量为指标进行筛分，然而该方法生产设备复杂、成本高，且生产率低，不适合实际应用的需求。
发明内容
针对目前分离聚合氯化钛优势水解形态成本高、操作复杂的问题，本发明提供一种分离纯化钛基优势水解形态的方法，易于操作，环境友好，产物混凝效果更加高效。
为实现上述目的，本发明采用如下技术方案。
一种分离纯化聚合氯化钛优势水解产物的方法，包括以下步骤：
（1）制备获得聚合氯化钛溶液；
（2）向聚合氯化钛溶液中加入硫酸盐溶液进行沉淀，固液分离，液体即为聚合氯化钛优势水解产物的溶液；
硫酸盐中硫酸根与聚合氯化钛中钛的摩尔比为1:1-8:1。
优选地，所述聚合氯化钛溶液采用慢速滴碱法制备获得。进一步地，所述慢速滴碱法的步骤如下：在搅拌条件下，向20%v/v的TiCl4溶液中滴加NaOH溶液至聚合氯化钛溶液碱化度为1.5（OH-/Ti=1.5）。
优选地，上述制备方法还包括熟化步骤：将聚合氯化钛溶液或聚合氯化钛优势水解产物的溶液，0-4℃静置熟化24 h。
所述硫酸盐选自硫酸钠或硫酸钾。
一种上述制备方法获得的聚合氯化钛优势水解产物。
上述聚合氯化钛优势水解产物可用于污水处理。
本发明的机理如下：
本发明采用硫酸盐沉淀法获得优势水解形态，通过硫酸根离子与聚合氯化钛中的钛单体或其某一聚合度的聚集体发生反应并生成沉淀，使其某一聚合度的产物达到纯化的目的。
本发明具有以下优点：
本发明通过控制不同的SO4 2-/Ti，确定硫酸根离子的最佳反应量，最终获得聚合氯化钛优势水解形态产物。相比通过分子量超滤的分离方法，易于操作，成本低，环境友好，易于获得富含优势水解形态的钛基盐混凝剂。
附图说明
图1是不同处理在各投加量下处理后水的浊度；
图2是不同处理在各投加量下处理后水的UV254去除率；
图3是不同处理在各投加量下处理后水的pH。
具体实施方式
下面结合实施例和附图对本发明做进一步说明，但本发明不受下述实施例的限制。
实施例1 聚合氯化钛优势水解产物的制备
1. 慢速滴碱法制备聚合氯化钛溶液
（1）在通风橱中，并在磁力搅拌作用和冰水浴的条件下，将20 mL质量分数为99%的纯四氯化钛溶液逐滴滴入到80 mL冰水中，滴加完毕后，持续搅拌3 h，制成体积分数为20%的四氯化钛初始液；
（2）在剧烈的磁力搅拌（1200 r/min）条件下，将NaOH溶液（200.0 g/L）逐滴滴加到步骤（1）制备的四氯化钛溶液中，在NaOH溶液滴加到四氯化钛溶液中后，会立刻产生白色物质，在前一滴的滴加产生的白色物质溶解消失之后继续滴加下一滴NaOH溶液；加入的氢氧化钠溶液与四氯化钛溶液的体积比为2:5；滴加完毕后，持续搅拌3 h，即得到采用慢速滴碱法制备的碱化度为1.5的聚合氯化钛（PTC）溶液，4℃静置熟化24 h后备用。
2. 硫酸沉淀法制备聚合氯化钛优势水解产物
（1）取几份等量的上述聚合氯化钛溶液，按照SO4 2-和Ti的摩尔比为1:1、4:1和8:1分别加入硫酸钠，搅拌反应8h，获得反应液；
（2）将反应液1500 r/min离心15 min，分离上清液和沉淀，沉淀加水溶解，获得上清液和沉淀溶解液均置于4℃静置熟化24 h；根据SO4 2-/Ti的摩尔比，上清液分别命名为S1:1、S4:1、S8:1，沉淀溶解液命名为P1:1、P4:1、P8:1。
应用例1 聚合氯化钛优势水解产物在水处理中的应用
取济南市黄河流域内的黄河水进行试验，黄河水样在波长254 nm下的吸光度为0.045±0.003 cm-1，浊度为1.22±0.56 NTU，pH为8.23±0.32。将实施例1、实施例2中制备的聚合氯化初始液及其分离纯化产物应用于地表水的水处理，按照Ti计算，投加量分别为5-55 mg/L，对比不同混凝剂对混凝效果的影响。
图1为不同处理在各投加量下处理后水的浊度，由图中可以看出，在不同SO4 2-/Ti的条件下得到的分离纯化产物，在最佳投加量下混凝出水剩余浊度都小于2 NTU；当SO4 2-/Ti为4:1和8:1时，上清液在高投加量下有返混现象。
图2为不同处理在各投加量下处理后水的UV254去除率，由图中可以看出，聚合氯化钛溶液在45 mg/L的投加量下混凝效果最佳，相比此时在不同SO4 2-/Ti的条件下得到的沉淀溶解液的混凝效果明显低于聚合氯化钛溶液；当SO4 2-/Ti为8:1时，沉淀溶解液虽在50 mg/L达到最佳投加量，但UV254去除率下降了10%左右；而上清液在5-30 mg/L的低投加量下比聚合氯化钛溶液的UV254去除率提升了20%左右。
图2为不同处理在各投加量下处理后水的pH，由图中可以看出，沉淀溶解液随着投加量的增加，混凝出水pH下降较平缓；而上清液随着投加量的增加，混凝出水pH下降较明显，且在最佳投加量下pH集中在3-4。
通过上述结果可知：在SO4 2-/Ti=1:1-8:1条件下，上清液中含有絮凝效果较好的产物，成功分离纯化了优势水解形态，相较聚合氯化钛溶液混凝效果更加高效。
Claims (7)
1.一种分离纯化聚合氯化钛优势水解产物的方法，其特征在于，包括以下步骤：
（1）制备获得聚合氯化钛溶液；
（2）向聚合氯化钛溶液中加入硫酸盐溶液进行沉淀，固液分离，液体即为聚合氯化钛优势水解产物的溶液；
硫酸盐中硫酸根与聚合氯化钛中钛的摩尔比为1:1-8:1。
2.根据权利要求1所述的方法，其特征在于，所述聚合氯化钛溶液采用慢速滴碱法制备获得。
3.根据权利要求2所述的方法，其特征在于，所述慢速滴碱法的步骤如下：在搅拌条件下，向20%v/v的TiCl4溶液中滴加NaOH溶液至聚合氯化钛溶液碱化度为1.5。
4.根据权利要求1所述的方法，其特征在于，步骤（1）和（2）还包括熟化步骤：将聚合氯化钛溶液或聚合氯化钛优势水解产物的溶液，0-4℃静置熟化24 h。
5.根据权利要求1所述的方法，其特征在于，所述硫酸盐选自硫酸钠或硫酸钾。
6.一种权利要求1-5任一所述的方法获得的聚合氯化钛优势水解产物。
7.一种权利要求6所述的聚合氯化钛优势水解产物在污水处理中的应用。
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| GB393264A (en) * | 1931-08-25 | 1933-05-25 | Howard Spence | Improvements in and relating to the preparation of titanium compounds |
| CN104724805A (zh) * | 2015-03-26 | 2015-06-24 | 山东大学 | 聚合硅酸聚合氯化钛无机高分子复合絮凝剂及其制备方法与应用 |
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