CN111606332A - 一种用电吸附提纯碳酸氢铵的方法 - Google Patents
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- C—CHEMISTRY; METALLURGY
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- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/26—Carbonates or bicarbonates of ammonium
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Abstract
本发明公开一种用电吸附提纯碳酸氢铵的方法,采用经过预处理的活性碳纤维作为电吸附模块的负极,对碳酸氢铵溶液进行电吸附;在电吸附过程中实时监测溶液的电导率,当电导率保持不变时停止电吸附;再将碳酸氢铵溶液冷冻干燥,得到高纯度碳酸氢铵。本发明获得的碳酸氢铵纯度高,采用冷冻干燥将碳酸氢铵溶液中的水分蒸发,使得碳酸氢铵的收率高,并且由于冷冻干燥的温度低,得到的碳酸氢铵不易分解,碳酸氢铵的收率高,还具有提纯过程快速、环保、无二次污染、设备简单、易操作、材料廉价易得等优点。
Description
技术领域
本发明涉及无机盐纯化技术领域,具体涉及一种用电吸附提纯碳酸氢铵的方法。
背景技术
碳酸氢铵(NH4HCO3)又称碳铵,是一种应用广泛的无机盐。在农业中可用作氮肥,适用于各种土壤,可同时提供作物生长所需的铵态氮和二氧化碳,能促进作物生长和光合作用,催苗长叶,可作追肥、也可作底肥直接施用。在工业中用作分析试剂,也用于合成铵盐和织物脱脂。作化学膨松剂,中国规定可用于各类需添加膨松剂的食品,按生产需要适量使用。还可以在食品中用作高级发酵剂,与碳酸氢钠合用可作面包、饼干、煎饼等膨松剂的原料,亦用作发泡粉末果汁的原料,还用于绿色蔬菜、竹笋等烫漂。以及医药及试剂,发酵粉亦以本品为主要成分,配以酸性物质。还可用于药学、生态治理等方面,可见碳铵具有良好的市场前景。因此制备高纯度碳酸氢铵具有重要的意义。
目前,高纯度碳酸氢铵的提纯主要采用结晶法。反应得到的碳酸氢铵悬浮液的固液比达到40%~70%,经过冷却,由于温度降低碳铵溶解度降低导致溶液过饱和,从而碳铵以晶体的形式析出,先沉淀,然后离心分离得到固体碳酸氢铵晶体干燥后得到产品。但是,结晶法制备碳酸氢铵存在以下不足:1、结晶过程中,碳酸氢铵的损失量大,在母液中还含有大量的碳酸氢铵,容易造成浪费。2、由于碳酸氢铵在36℃以上分解为二氧化碳、氨和水,60℃可分解完,而结晶过程中温度较高,析出的碳酸氢铵容易分解,导致碳酸氢铵的收率降低,碳酸氢铵的制备成本高,不利于工业化生产。3、传统的热风干燥损失较大。4、通过结晶法提纯的碳酸氢铵中含有金属离子等杂质,在结晶形成的碳酸氢铵中难以去除,使得碳酸氢铵的纯度不高。
发明内容
针对现有技术存在的上述不足,本发明的目的在于解决采用结晶法制备的碳酸氢铵容易分解、纯度不高的问题。
为了解决上述技术问题,本发明采用如下技术方案:
一种用电吸附提纯碳酸氢铵的方法,采用经过预处理的活性碳纤维作为电吸附模块的负极,石墨板作为电吸附模块的正极,对碳酸氢铵溶液进行电吸附;在电吸附过程中实时监测溶液的电导率,当电导率保持不变时停止电吸附;再将碳酸氢铵溶液冷冻干燥,得到高纯度碳酸氢铵。
其中,所述活性碳纤维的预处理方法为:将活性碳纤维用适量的丙酮洗涤浸泡后,用蒸馏水清洗2~3次;再用盐酸浸泡,同时超声辅助活化;最后用蒸馏水清洗至中性,真空抽滤,80~130℃真空干燥4~10 h得到活性碳纤维电极。
优选,所述丙酮洗涤浸泡的时间为2~4 h。所述盐酸的浓度为0.5~3 mol/L,超声功率为100~500W,频率为20~40kHz,超声时间为15~60min。
进一步,所述碳酸氢铵溶液的浓度为10%至饱和溶液。所述电吸附过程中通电电压为1.2~10V,极板间距为8~30 cm;碳酸氢铵溶液的流量为20~60 mL/min。
进一步,所述冷冻干燥的温度为- 40~-5℃。
进一步,还包括活性碳纤维电极脱附再生的步骤;将施加在电吸附模块上的电压短路或者交换电极,放入去离子水中,使活性碳纤维电极进行脱附,直到水溶液中的电导率恢复到初始值,取出活性碳纤维置于超声波中超声得到脱附再生电极,用于重复吸附。
相比现有技术,本发明具有如下有益效果:
1、本发明采用电吸附提纯碳酸氢铵的方法,由于电吸附的方式提纯碳酸氢铵溶液,然后采用冷冻干燥的方式制得碳酸氢铵,有效解决了采用结晶法制备碳酸氢铵时,碳酸氢铵容易分解,且制备的碳酸氢铵中含有金属离子、纯度不高、不能满足高纯度的要求的问题,并且快速、环保、无二次污染。
2、本发明根据同性相吸的原理,碳酸氢铵溶液中的杂质被吸附到作为负极的活性碳纤维上,从而实现碳酸氢铵溶液的提纯;并且采用冷冻干燥将碳酸氢铵溶液中的水分蒸发,使得碳酸氢铵的收率高,并且由于冷冻干燥的温度低,得到的碳酸氢铵不易分解,碳酸氢铵的损失量小。
3、采用活性碳纤维作为电吸附模块的电极,设备简单、易操作、材料便宜易得,工业上可以连续操作,活性碳纤维可循环使用,且制作成本低廉、效率高。
4、本发明还提供活性碳纤维电极脱附再生的步骤,经过吸附后的活性碳纤维电极达到饱和后,通过电机脱附即可实现再生,因此能够循环使用,降低碳酸氢铵的提纯成本。
附图说明
图1为本发明实施例5中的活性碳纤维循环吸附次数与吸附率和脱附率的关系图。
具体实施方式
下面将结合附图和实施例对本发明作进一步说明。
实施例1:一种用电吸附提纯碳酸氢铵的方法,包括以下步骤:
(1)活性碳纤维的预处理:将活性碳纤维剪成10 cm × 5 cm大小,用丙酮浸泡2h,用蒸馏水清洗2~3次。用1mol/L的盐酸浸泡,同时放入功率为100W的超声波中超声30min,然后用大量的蒸馏水清洗,直至pH值为中性,真空抽滤,85℃真空干燥8h。
(2)碳酸氢铵的提纯:将步骤(1)处理后的活性碳纤维作为电吸附模块的负极、石墨板作为电吸附模块的正极。将碳酸氢铵配置成10%的溶液,加入到电吸附槽中进行电吸附;其中,碳酸氢铵溶液的流量为30mL/min,通电电压为2.0V,极板间距10cm,吸附时间30min。当电导率保持不变时,电吸附后的碳酸氢铵溶液经冷冻干燥得到高纯度碳酸氢铵。
碳酸氢铵纯度测试采用国标GB T 6276.1-2008检测,原碳酸氢铵纯度为98.4±0.03%,电吸附后碳酸氢铵纯度为99.96%。
实施例2~4:一种用电吸附提纯碳酸氢铵的方法,包括以下步骤:
(1)活性碳纤维的预处理如实施例1中(1)。
(2)碳酸氢铵的提纯:将步骤(1)处理后的活性碳纤维作为电吸附模块的负极、石墨板作为电吸附模块的正极。将碳酸氢铵配置成溶液,加入到电吸附槽中进行电吸附;电吸附的条件如下表所示,电吸附结束后的碳酸氢铵溶液经冷冻干燥得到高纯度碳酸氢铵,结果如下表所示。
碳酸氢铵溶液浓度 | 碳酸氢铵溶液流量 | 通电电压 | 极板间距 | 时间 | 碳酸氢铵纯度 | |
实施例1 | 10% | 30mL/min | 2.0V | 10cm | 30min | 99.960% |
实施例2 | 10% | 30mL/min | 10.0V | 15cm | 20min | 99.996% |
实施例3 | 35% | 30mL/min | 2.0V | 10cm | 30min | 99.950% |
实施例4 | 35% | 60mL/min | 10.0V | 15cm | 20min | 99.993% |
实施例5:活性碳纤维电极的脱附再生,包括以下步骤:
将实施例1中的活性碳纤维电极达到吸附饱和后,将施加在电吸附模块上的电压短路,使活性碳纤维电极进行脱附,直到溶液中的电导率恢复到初始值,取出活性碳纤维置于超声波中,超声功率为100W,超声5min,得到脱附再生电极。
实施例6:活性碳纤维的循环电吸附
将实施例5中脱附再生的活性碳纤维电极再次用于电吸附提纯碳酸氢铵,碳酸氢铵溶液的浓度和流量,以及电吸附条件与实施例1相同。
参见附图1,将脱附后的活性碳纤维安装到吸附槽中进行第一次循环吸附实验后,活性碳纤维的吸附率为56.78%,经过五次循环吸附脱附实验后去除率仅降低了8.56%。
其中,吸附率的计算方法为:;
脱附率的计算方法:;
其中,m 初为未吸附时的活性炭纤维的质量,m 平为活性炭纤维吸附平衡时的质量。
可见,采用本发明提纯碳酸氢铵具有纯度高、收率高和损失量小等优点,尤其适合在工业上推广使用。本发明中的活性炭纤维经过处理后具有很好的再生性能,有利于工业生产中降低成本。
最后需要说明的是,以上实施例仅用以说明本发明的技术方案而非限制技术方案,本领域的普通技术人员应当理解,那些对本发明的技术方案进行修改或者等同替换,而不脱离本技术方案的宗旨和范围,均应涵盖在本发明的权利要求范围当中。
Claims (8)
1.一种用电吸附提纯碳酸氢铵的方法,其特征在于,采用经过预处理的活性碳纤维作为电吸附模块的负极,石墨板作为电吸附模块的正极,对碳酸氢铵溶液进行电吸附;在电吸附过程中实时监测溶液的电导率,当电导率保持不变时停止电吸附;再将碳酸氢铵溶液冷冻干燥,得到高纯度碳酸氢铵。
2.根据权利要求1所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述活性碳纤维的预处理方法为:将活性碳纤维用适量的丙酮洗涤浸泡后,用蒸馏水清洗2~3次;再用盐酸浸泡,同时超声辅助活化;最后用蒸馏水清洗至中性,真空抽滤,80~130℃真空干燥4~10 h得到活性碳纤维电极。
3.根据权利要求2所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述丙酮洗涤浸泡的时间为2~4 h。
4.根据权利要求2所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述盐酸的浓度为0.5~3 mol/L,超声功率为100~500W,频率为20~40kHz,超声时间为15~60min。
5.根据权利要求1所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述碳酸氢铵溶液的浓度为10%至饱和溶液。
6.根据权利要求1所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述电吸附过程中通电电压为1.2~10V,极板间距为8~30 cm;碳酸氢铵溶液的流量为20~60 mL/min。
7.根据权利要求1所述用电吸附提纯碳酸氢铵的方法,其特征在于,所述冷冻干燥的温度为- 40~-5℃。
8.根据权利要求1~7任一所述用电吸附提纯碳酸氢铵的方法,其特征在于,还包括活性碳纤维电极脱附再生的步骤;将施加在电吸附模块上的电压短路或者交换电极,放入去离子水中,使活性碳纤维电极进行脱附,直到水溶液中的电导率恢复到初始值,取出活性碳纤维置于超声波中超声得到脱附再生电极,用于重复吸附。
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