CN108841814A - 基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法 - Google Patents
基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法 Download PDFInfo
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Abstract
本发明属于缓释碳材料技术领域,公开了一种基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法,鉴于淀粉、聚乙烯醇、海藻酸钠价格低廉,且均具有较好的亲水性,两者可充分地共混,形成良好的缓释性和生物降解性,本发明以聚乙烯醇、海藻酸钠为骨架和包埋剂,以淀粉为碳源,制备缓释碳材料,附加和调节α‑淀粉酶,控制淀粉分子的水解程度,协调释碳速率与反硝化过程。在该过程中,该缓释碳材料的有效控制可以减少释碳过程造成的有机物污染。以期获得较长的使用周期和较好的脱氮效果。在制得新型缓释碳源后,对其进行脱氮工艺的运行特性研究,为其工程应用提供技术参考。
Description
技术领域
本发明属于缓释碳材料技术领域,尤其涉及一种基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法。
背景技术
目前,业内常用的现有技术是这样的:异养反硝化是常见的反硝化过程,也是去除硝酸盐最有效的一种方法。异养反硝化过程需要充足的有机碳作为电子供体,需要外加碳源。现有常用的外加碳源,主要有两大类:以甲醇、乙醇、乙酸、葡萄糖为主的传统碳源,以及以天然纤维素类物质为主的可生物降解的聚合物以及合成聚合物,如PHB(聚β-羟基丁酸)、PHBV(聚β-羟基丁酸戊酸醋)等。但是,传统碳源存在投加过量的隐患,会影响出水水质,需要精确控制投加量以及投加过程,合成的聚合物费用较高,且碳源释放不能得到有效控制,会带来较高的DOC溶解问题。常用的液态有机碳源如甲醇、乙醇等虽然有良好的供碳效果,但是其在经济性和安全性方面均存在不足,并且甲醇的毒性会造成二次污染。因此,制备价格低廉、性能优越的新型固体缓释碳源成为污水反硝化脱氮的关键环节。
综上所述,现有技术存在的问题是:
(1)液相碳源的消耗快,耗损大,必须经常增补从而花费高,若不慎添加过量的有机碳,导致反应不完全而造成二次污染,在实际应用中造成诸多不便;
(2)现有的释碳材料,大多以聚乙烯醇或者海藻酸钠为单独的碳源载体,本项技术中采用聚乙烯醇和海藻酸钠为碳源载体,在保证其释碳材料稳定性的同时,进一步保证其材料的制备;
(3)在现有的释碳材料制备中,大多以淀粉为碳源,但是释碳材料的速率不能得到很好的控制,在本发明中,添加α-淀粉酶,用于控制和调节释碳材料的释放速率。
解决上述技术问题的难度和意义:
(1)为释碳材料的进一步研究提供数据支撑和理论知识;
(2)在现有基础上,添加α-淀粉酶,控制和调节释碳材料的释放速率,为实际工程中精准化应用提供数据支撑。
(3)研制出合适稳定的有机碳源载体,能高效、持续地应用于污水中硝酸盐的污染修复。
发明内容
针对现有技术存在的问题,本发明提供了一种基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法。
本发明是这样实现的,一种基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法,所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法以聚乙烯醇、海藻酸钠为骨架和包埋剂,以淀粉为碳源,制备缓释碳材料,附加和调节α-淀粉酶,控制淀粉分子的水解程度,协调释碳速率与反硝化过程。
进一步,所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法包括以下步骤:
步骤一,将海藻酸钠、聚乙烯醇、无菌水水浴加热65~75摄氏度溶解;
步骤二,粘稠状固定化材料混合液,添加α-淀粉酶,得到缓释碳材料混合体系;
步骤三,使用注射器,得到饱和硼酸溶液,形成均匀小球。
本发明的另一目的在于提供一种由所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法制备的基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料。
本发明的另一目的在于提供一种所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的测定方法,所述测定方法使用的拟合模型公式为:
K=3.34-1.55A+1.01B-2.12C-1.07AB-0.53AC-0.50BC+4.26A2+1.44B2+2.59C2
式中:A为聚乙烯醇的浓度;B为淀粉的浓度;C为淀粉酶的浓度。
综上所述,本发明的优点及积极效果为:
(1)用此技术制备的缓释碳材料具有一定硬度和稳定性,在实验运行中保持稳定,不易发生溶解分离等现象;
(2)用此技术制备的缓释碳材料具有较高的释碳效果,其中10号实验制备缓释碳材料可以在运行10h,其体系中COD为98.78mg/(g·L),运行20h后,体系中COD达到122.36mg/(g·L),之后稳定在此水平。17号实验制备的缓释碳材料在运行70h后,体系中COD达到130.23mg/(g·L),并稳定在此水平。除此之外,在实验运行60h以内,10号实验制备缓释碳材料效率最高;60h以后,17号实验制备缓释碳材料效率最高。具体各组实验结果如下图2所示,10号和17号实验缓释碳材料释碳效果图及对比图分别为图3、图4和图5。
(3)利用响应曲面法对材料进行分析,将聚乙烯醇浓度、淀粉浓度和α-淀粉酶活性作为自变量,材料传质系数作为因变量,对模型进行拟合,发现模型拟合度高,同时对三维立体图进行分析,发现随着浓度的升高,聚乙烯醇浓度、淀粉浓度和α-淀粉酶的活性都对释碳材料的释碳性能产生影响,利用DesignExpert软件优化筛选,得到的最优配比为:聚乙烯醇浓度为4.22%,淀粉浓度为9.29%,α-淀粉酶活性为0.03U/g,传质系数值为2.92mg/(h·g·L),该数值与实验17组相吻合。具体响应曲面分析图如下,拟合模型公式为:
K=3.34-1.55A+1.01B-2.12C-1.07AB-0.53AC-0.50BC+4.26A2+1.44B2+2.59C2
式中:A为聚乙烯醇的浓度;B为淀粉的浓度;C为淀粉酶的浓度。
响应面二次模型的方差分析如表1所示。可知,模型的F值为108.73,P值小于0.0001,表示回归模型显著,回归效果比较理想,表明该模型是有效的,回归决定系数R2的值为0.9929,表示回归方差预测的可靠性达99.29%,校正决定系数R2(Adj)的值为0.9838,R2和R2(Adj)的值非常相近,与1相比差距很小,说明该方程拟合效果好。变异系数CV的值为6.15%,精密度(AdeqPrecision)的值为29.262,表明了该实验的变异数概率小,精确度相较来说高,模型的拟合度好。
因此,通过实验数据及模型拟合,最终确定最佳缓释碳材料配比为17号实验。但是,在实际应用中,可以根据反应器运行时间的长短以及规模选择10号或17号合适的缓释碳材料作为碳源。
表1响应面二次模型的方差分析表
附图说明
图1是本发明实施例提供的缓释碳材料制备方法流程图;
图2是本发明实施例提供的17组缓释碳材料在不同运行时间的释碳情况;
图3是本发明实施例提供的试验10号缓释碳材料效果图;
图4是本发明实施例提供的17号实验缓释碳材料效果图;
图5是本发明实施例提供的10号和17号缓释碳材料效果对比图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅用以解释本发明,并不用于限定本发明。
下面结合附图对本发明的应用原理作详细的描述。
如图1所示,本发明实施例提供的基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法包括以下步骤:
步骤一,将海藻酸钠、聚乙烯醇、无菌水水浴加热65~75摄氏度溶解;
步骤二,粘稠状固定化材料混合液,添加α-淀粉酶,得到缓释碳材料混合体系;
步骤三,使用注射器,得到饱和硼酸溶液,形成均匀小球。
下面结合实验对本发明的应用效果做详细的描述。
(1)实验设计
选择PVA浓度、淀粉浓度以及α-淀粉酶浓度三因素,通过查阅国内外文献和预实验,设定SA浓度为0.4%,PVA(浓度水平2%、4%和6%),淀粉(8%、10%和12%)以及α-淀粉酶(0、0.03、0.06),利用响应曲面法(Response surfacemethodology,RSM)进行试验设计,研究分析各个因素之间联系、确定最佳缓释碳材料配比,并研究三因素对缓释碳材料效率的影响。具体实验参数设计见表2和实验设计见表3如下:
表2三因素选择与水平
表3RSM三因素三水平实验设计安排
(2)17组缓释碳材料小球的制备
首先,配置含4%CaCl2的饱和硼酸溶液备用,然后按照实验设计称取一定量的聚乙烯醇、海藻酸钠、淀粉和α-淀粉酶,并加入定量的二次蒸馏水配制成溶液,混合均匀后置于60℃~80℃水浴锅中加热,当搅拌混合均匀后,用注射器滴加到盛装4%CaCl2的饱和硼酸溶液的玻璃器皿中浸泡至少24h,使其充分与饱和溶液接触,吸附其中的钙离子,形成球状颗粒,并用封口膜将其密封。当吸收了充足的钙离子后,用二次蒸馏水将其洗净后置于贴好标签的玻璃器皿,在4℃的冰箱中保存备用。实施流程为图1。
(3)17组缓释碳材料小球的性能评定:
具体实验结果如图2-“17组缓释碳材料在不同运行时间的释碳情况”所示,从实验结果中,可得到试验10号和17号实验制备的缓释碳材料的释碳性能较好。具体释碳材料配比见表4和释碳情况见图3、图4.
表4实验结果优选缓释碳材料配比
以上所述仅为本发明的较佳实施例而已,并不用以限制本发明,凡在本发明的精神和原则之内所作的任何修改、等同替换和改进等,均应包含在本发明的保护范围之内。
Claims (4)
1.一种基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法,其特征在于,所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法以聚乙烯醇、海藻酸钠为骨架和包埋剂,以淀粉为碳源,制备缓释碳材料,附加和调节α-淀粉酶,控制淀粉分子的水解程度,协调释碳速率与反硝化过程。
2.如权利要求1所述的基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法,其特征在于,所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法包括以下步骤:
步骤一,将海藻酸钠、聚乙烯醇、无菌水水浴加热65~75摄氏度溶解;
步骤二,粘稠状固定化材料混合液,添加α-淀粉酶,得到缓释碳材料混合体系;
步骤三,使用注射器,得到饱和硼酸溶液,形成均匀小球。
3.一种由权利要求1~2任意一项所述基于聚乙烯醇、海藻酸钠和淀粉制备缓释碳材料的方法制备的缓释碳材料。
4.一种如权利要求3所述缓释碳材料的测定方法,其特征在于,所述测定方法使用的拟合模型公式为:
K=3.34-1.55A+1.01B-2.12C-1.07AB-0.53AC-0.50BC+4.26A2+1.44B2+2.59C2
式中:A为聚乙烯醇的浓度;B为淀粉的浓度;C为淀粉酶的浓度。
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