CN113331208B - 一种稳定型纳米银钛悬浮液及其的制备方法 - Google Patents
一种稳定型纳米银钛悬浮液及其的制备方法 Download PDFInfo
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Abstract
本发明属于纳米材料领域,具体为一种稳定型纳米银钛悬浮液及其制备方法。该悬浮液由纳米银、纳米二氧化钛、添加剂、可溶淀粉、酵母菌、苯磺酸钠和水构成。悬浮液中纳米银和纳米二氧化钛能均匀长时间地分散在水中悬浮,其粒子的悬浮时间可达60h以上。其制备方法为:水中加入添加剂充分搅拌得到分散液A,在定量的分散液A中加入可溶淀粉、酵母菌和苯磺酸钠充分搅拌,得到分散液B;在定量的分散液A中加入乙醇和碳酸钠充分搅拌得到溶液C;将硝酸银溶液和钛酸四丁酯分别滴加到溶液C中,将反应物水洗三遍后真空加热到200‑500℃,得到纳米二氧化钛和纳米银,加入到定量的分散液B中,超声分散10‑20min。该制备方法简捷,绿色环保。
Description
技术领域
本发明属于纳米材料领域,具体涉及一种稳定型纳米银钛悬浮液及其的制备方法。
背景技术
纳米银是粉末状银单质,粒径小于100nm。纳米银粒子除了在微电子领域占有极其重要的地位外,在杀菌领域也有重要的应用。研究发现,粒径越小,杀菌性能越强。纳米银粒径大多在50纳米以下,对大肠杆菌、淋球菌、沙眼衣原体等几十种致病微生物都有强烈的抑制和杀灭作用,而且不会产生耐药性。迄今为止,由于拥有优秀的抗菌效果,纳米银仍然被广泛应用在婴儿奶瓶、玩具、牙刷、牙膏、空气净化器等产品。用纳米银和精梳棉纤维制成的棉袜,具备很好的抗菌防臭的效果。
纳米级二氧化钛,直径在100纳米以下,具有抗线、抗菌、自洁净、抗老化性能,可用于化妆品、功能纤维、塑料、油墨、涂料、油漆、精细陶瓷等领域。纳米银和纳米二氧化钛等纳米粒子的水性悬浮液具有很大的优点,但是纳米粒子比表面大,表面能高,在水中很容易自动团聚下沉。如何解决纳米粒子在水中能够长时间悬浮而不沉降,一直为国内外所关注。
专利公开号CN105001433B提出了一种壳聚糖纳米粒悬浮液的制备方法,该方法需要高压匀质处理,不仅难度大,而且纳米粒子悬浮的时间不长。专利公告号CN104190279A公开了一种纳米二氧化钛分散液的制备方法,该方法是将纳米二氧化钛加入到去离子水中,进行磁力搅拌,再加入聚丙酰胺PAAM作为絮凝剂并调节搅拌速度和时间,可获得所述纳米二氧化钛分散液。该方法得到的悬浮液虽然有一定的分散性,但是不长时间后纳米粒子还是很快发生了团聚下沉的现象。
发明内容
为解决现有技术的上述问题,本发明提供一种稳定型纳米银钛悬浮液及其制备方法,该悬浮液中的纳米银和纳米二氧化钛具有良好的杀菌和光催化效果,能均匀而且长时间地分散在水中形成悬浮液,纳米粒子悬浮的时间可达到60h。该悬浮液无毒、无害、无味,制备方法简捷,而且在整个制备工艺过程中都绿色环保。
为此本发明提供一种稳定型纳米银钛悬浮液,包括:纳米银、纳米二氧化钛、添加剂、可溶淀粉、酵母菌、苯磺酸钠和水构成。所述纳米银的含量为0.01~10wt%;所述纳米二氧化钛的含量为0.5~8wt%;所述添加剂的含量为0.002~0.009wt%;所述可溶淀粉的含量为0.5~9wt%;所述酵母菌的含量为0.1~6wt%;所述苯磺酸钠的含量为0.04~0.12wt%;其余为水。
进一步的,所述纳米银的粒度为20-60nm。纳米银的粒度在此范围内悬浮性能最好且杀菌效果好,粒度小于20nm时制备复杂且成本高,大于60nm时杀菌效果大大下降。
进一步的,所述纳米二氧化钛的粒度为5-80nm。纳米二氧化钛的粒度在此范围内光催化效果最佳,粒度小于5nm时制备条件要求和成本高,大于80nm时长期悬浮性较差。
进一步的,所述的添加剂为甘露糖和烯丙基聚氧乙烯醚的混合物,所述甘露糖的含量为19-34%。这种含量比能够使物料充分而均匀的分散,悬浮时间长。
进一步的,所述的一种稳定型纳米银钛悬浮液的制备方法,制备时包括如下步骤:
(1)将添加剂加入到一定量的水中,充分搅拌,得到分散液A。
(2)将可溶淀粉、酵母菌和苯磺酸钠加入到一定量的分散液A中,充分搅拌,得到分散液B。
(3)在一定量的分散液A中加入乙醇(占分散液A质量的6-20%)和碳酸钠(占分散液质量的3-10%),充分搅拌,得到溶液C。
(4)将硝酸银溶液和钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到200-500℃,便可得到纳米二氧化钛和纳米银,二者均匀地混合在一起。
(5)将所述纳米银和纳米二氧化钛加入到一定量的分散液B中,超声分散10-20min,便可得到该稳定型纳米银钛悬浮液。
有益效果
该纳米银钛悬浮液中的纳米银和纳米二氧化钛具有良好的杀菌和光催化效果,能均匀而且长时间地分散在水中成悬浮液,纳米粒子的悬浮时间可达到60h。并且该悬浮液无毒、无害、无味,制备方法简捷,而且在整个制备工艺过程中都绿色环保。
具体实施方式
下面的实施例只是用于详细说明本发明,并不以任何方式限制发明的保护范围。
实施例1:
(1)将0.0028g添加剂加入到98g水中,充分搅拌,得到分散液A。
(2)将1.2g可溶淀粉、0.37g酵母菌和0.06g苯磺酸钠加入到98g分散液A中,充分搅拌,得到分散液B。
(3)在90g分散液A中加入12g乙醇和9.2g碳酸钠,充分搅拌,得到溶液C。
(4)将质量百分比浓度为1%硝酸银溶液80g和3g钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到200℃,便可得到纳米二氧化钛和纳米银。纳米银的平均粒度为20nm,纳米二氧化钛的平均粒度为5nm。
(5)将所述纳米银和纳米二氧化钛加入到98g分散液B中,超声分散10min,便可得到该稳定型纳米银钛悬浮液。其中纳米银的含量为0.5%,纳米二氧化钛的含量为0.7%。
实施例2:
(1)将0.0022g添加剂加入到98g水中,充分搅拌,得到分散液A。
(2)将1g可溶淀粉、0.3g酵母菌和0.04g苯磺酸钠加入到98g分散液A中,充分搅拌,得到分散液B。
(3)在90g分散液A中加入10g乙醇和6g碳酸钠,充分搅拌,得到溶液C。
(4)将质量百分比浓度为1%硝酸银溶液100g和6g钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到300℃,便可得到纳米二氧化钛和纳米银。纳米银的平均粒度为30nm,纳米二氧化钛的平均粒度为20nm。
(5)将所述纳米银和纳米二氧化钛加入到98g分散液B中,超声分散13min,便可得到该稳定型纳米银钛悬浮液。其中纳米银的含量为0.6%,纳米二氧化钛的含量为1.4%。
实施例3:
(1)将0.004g添加剂加入到100g水中,充分搅拌,得到分散液A。
(2)将2g可溶淀粉、0.7g酵母菌和0.08g苯磺酸钠加入到100g分散A中,充分搅拌,得到分散液B。
(3)在100g分散液A中加入14g乙醇和8g碳酸钠,充分搅拌,得到溶液C。
(4)将质量百分比浓度为2%硝酸银溶液100g和10g钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到450℃,便可得到纳米二氧化钛和纳米银。纳米银的平均粒度为36nm,纳米二氧化钛的平均粒度为41nm。
(5)将所述纳米银和纳米二氧化钛加入到96.5g分散液B中,超声分散16min,便可得到该稳定型纳米银钛悬浮液。其中纳米银的含量为1.2%,纳米二氧化钛的含量为2.3%。
实施例4:
(1)将0.0032g添加剂加入到94.7g水中,充分搅拌,得到分散液A。
(2)将6g可溶淀粉、3g酵母菌和0.12g苯磺酸钠加入到94.7g分散A中,充分搅拌,得到分散液B。
(3)在90g分散液A中加入11g乙醇和5g碳酸钠,充分搅拌,得到溶液C。
(4)将质量百分比浓度为3%硝酸银溶液100g和15g钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到500℃,便可得到纳米二氧化钛和纳米银。纳米银的平均粒度为51nm,纳米二氧化钛的平均粒度为57nm。
(5)将上述纳米银和纳米二氧化钛加入到94.7g分散液B中,超声分散18min,便可得到该稳定型纳米银钛悬浮液。其中纳米银的含量为1.8%,纳米二氧化钛的含量为3.5%。
实施例5:
(1)将0.005g添加剂加入到100g水中,充分搅拌,得到分散液A。
(2)将5g可溶淀粉、5g酵母菌和0.10g苯磺酸钠加入到100g分散A中,充分搅拌,得到分散液B。
(3)在100g分散液A中加入17g乙醇和9g碳酸钠,充分搅拌,得到溶液C。
(4)将质量百分比浓度为4%硝酸银溶液100g和24g钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌。反应结束后,将反应物及产物用水洗三遍后真空加热到400℃,便可得到纳米二氧化钛和纳米银。纳米银的平均粒度为60nm,纳米二氧化钛的平均粒度为80nm。
(5)将上述纳米银和纳米二氧化钛加入到92g分散液B中,超声分散20min,便可得到该稳定型纳米银钛悬浮液。其中纳米银的含量为2.4%,纳米二氧化钛的含量为5.6%。
下面将实验中测得的实施例1-实施例5的纳米粒子平均粒度和悬浮时间,通过下表列举出来:
实施例1-4纳米粒子平均粒度和悬浮时间表
纳米银平均粒度(nm) | 纳米二氧化钛平均粒度(nm) | 悬浮时间(h) | |
实施例1 | 20 | 5 | 76 |
实施例2 | 30 | 20 | 73 |
实施例3 | 46 | 38 | 70 |
实施例4 | 51 | 57 | 67 |
实施例5 | 60 | 80 | 62 |
以上虽然结合实施例对本发明作了详细的说明,但是所述技术领域的技术人员能够理解,在不脱离本发明宗旨的前提下,在权利要求保护范围内,还可以对上述实施例进行变更或改变等。
Claims (1)
1.一种稳定型纳米银钛悬浮液,其特征在于:所述悬浮液是由纳米银、纳米二氧化钛、添加剂、可溶淀粉、酵母菌、苯磺酸钠和水构成;所述纳米银的含量为0.01~10 wt%;所述纳米二氧化钛的含量为0.5~8 wt% ;所述添加剂的含量为0.002~0.009 wt%;所述可溶淀粉的含量为0.5~9 wt%;所述酵母菌的含量为0.1~6wt%;所述苯磺酸钠的含量为0.04~0.12 wt%;其余为水;
所述纳米银的粒度为20-60 nm;
所述纳米二氧化钛的粒度为5-80 nm;
所述的添加剂为甘露糖和烯丙基聚氧乙烯醚的混合物,所述甘露糖的含量为19-34% ;
所述的一种稳定型纳米银钛悬浮液的制备方法,包括如下步骤:
(1)将添加剂加入到一定量的水中,充分搅拌,得到分散液A;
(2)将可溶淀粉、酵母菌和苯磺酸钠加入到一定量的分散液A中,充分搅拌,得到分散液B;
(3)在一定量的分散液A中加入占分散液A质量6-20%的乙醇和占分散液A质量3-10%的碳酸钠,充分搅拌,得到溶液C;
(4)将硝酸银溶液和钛酸四丁酯分别装在两个滴管中,同时滴加到溶液C中,控制滴加速度,一边滴加,一边搅拌; 反应结束后,将反应物及产物用水洗三遍后真空加热到200-500℃,便可得到纳米二氧化钛和纳米银,二者均匀地混合在一起;
(5)将所述纳米银和纳米二氧化钛加入一定量的分散液B中,超声分散10-20min,便可得到该稳定型纳米银钛悬浮液。
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