CN106749924B - 一种可降解玉米芯生物质保水剂的制备方法 - Google Patents
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Abstract
本发明公开了一种可降解玉米芯生物质保水剂的制备方法，是以改性玉米芯、丙烯酰胺为主要原料，加入交联剂、引发剂，通过反应交联聚合而得。本发明采用废弃的玉米芯为原料，大大降低了保水剂的生产成本；充分利用改性玉米芯的表面以及内部有很多细微孔的特殊结构特征，制备可降解保水剂具有很好的吸水性能和降解性能。
Description
技术领域
本发明属于生物质材料技术领域，涉及保水剂，尤其涉及一种可降解玉米芯生物质保水剂的制备方法。
背景技术
我国是农业大国，植物纤维资源丰富，玉米芯是玉米脱去籽粒后的穗轴，一般占玉米穗的20-30%左右。2015/16年度中国玉米产量预计为2.25亿吨，可以副产4000万吨的玉米芯，每年数千万吨的玉米芯被烧掉，既浪费资源又污染环境。对玉米芯深加工不但可以提高玉米副产品的利用价值，又具有较高的社会经济效益和广阔的发展前景。玉米芯含有丰富的纤维素(32%-36%),半纤维素(35%-40%)和木质素(17%-20%)，玉米芯粉本身具有海绵结构可吸收四倍于自重的液体，是一种很有发展的吸附材料资源，而且具有许多毛细管作用的纤维状物质。但是通常都是直接将玉米芯粉碎晒干，直接糊化、加交联剂、引发剂等制备可降解生物质保水剂，采用此方法制备的保水剂吸水能力有限，保水时间有限，在干旱的地区使用时，用量大，成本高。
发明内容
为了解决现有技术中存在的上述问题，本发明的目的是提供一种利用改性玉米芯制备可降解生物质保水剂的方法。
本发明采用如下技术方案：
本发明的一种可降解玉米芯生物质保水剂的制备方法，具体包括以下步骤：
A.改性玉米芯：先用粉碎机将干燥的玉米芯粉碎至5-500目，经微波辐射100-300w改性5-20min，然后酸酐改性；所述酸酐改性是将微波辐射后的玉米芯投入0.1-1mol/L酸酐溶液中，在50-90℃下改性4-10h，然后用水冲洗2-3次，烘干，备用；
B.制备可降解生物质保水剂：将步骤A中二次改性后的玉米芯粉末分散于水中，在30-80℃糊化0.5-1h；然后向该分散体系中加入丙烯酰胺，搅拌均匀，在氮气保护下，加入交联剂、引发剂至凝胶生成，最后用乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂。
所述的酸酐溶液是甲酸酐、乙酸酐、邻苯二甲酸酐、马来酸酐中的任意一种。
所述改性玉米芯粉末与丙烯酰胺的质量比为：1:5-1:10。
所述交联剂为：N，N-二甲基甲酰胺、N,N-亚甲基双丙烯酰胺、丙三醇、双氧水中的任意一种。
所述引发剂为：过硫酸铵、过硫酸铵-亚硫酸氢钠、过硫酸钾、2-酮戊二酸中的任意一种。
优选的，所述改性玉米芯粉末与交联剂的质量比为：100:0.5-100:5。
优选的，所述改性玉米芯粉末与引发剂的质量比为：100:1-100:10。
本发明的优点是：
1. 本发明采用废弃的玉米芯为原料，大大降低了保水剂的生产成本；本发明是以改性玉米芯、丙烯酰胺为主要原料，加入交联剂、引发剂，通过反应交联聚合而得。本发明的玉米芯通过两次改性，首先通过对玉米芯微波照射改性，严格控制时间和微波照射强度，使玉米芯内水分蒸发、且通过微波彻底打通玉米芯大分子的内部通道，使其内部通到更为疏松和通畅，吸附率增加。
2.本发明在微波照射一次改性后，再采用酸酐对玉米芯进行二次改性，使酸酐与玉米芯的纤维素、半纤维素和木质素上的羟基发生反应，通过化学反应使玉米芯带有更强和更多的亲水基团，同时还有造孔的作用，进一步增大微孔和提高孔隙率。对玉米芯改性，玉米芯结构具有更多的微孔和孔隙率，吸附性能大大提高。通过本发明的方法制备的保水剂与通用的玉米芯保水剂相比具有良好的吸水性、保水性和降解性能，是一种绿色环保的保水剂。
3.本发明实施例中制备的玉米芯生物质保水剂的吸水率可达到320g/g以上，吸0.9％盐水率为81 g/g以上。通过高吸水树脂能够明显抑制土壤表面的水分蒸发，随着树脂施用量的增加，抑制蒸发作用增强。
本发明保水剂的表征：
1.红外表征
在670-1048cm-1出现的是玉米芯的-CH2-振动吸收峰，说明玉米芯接枝了丙烯酸。
2.热稳定性表征
图2为保水剂热稳定性曲线。从图2可以看出，改性玉米芯保水剂从50℃到410 ℃失重率为71%，400-700℃失重率基本稳定，这是由于保水剂形成了网状结构，使保水剂具有较好的稳定性。
3.扫描电镜表征
图3为保水剂的微观形貌扫描电镜照片。从照片可以看出，改性玉米芯保水剂吸水前有大量的微孔结构，便面粗糙，比表面积大。从图4可以看出，与现有的玉米芯为主料生产的保水剂相比本发明制备的保水剂具有大量的微孔，大量的微孔可以容纳更多的水，吸水后比较饱满。
附图说明
图1. 本发明保水剂的红外光谱图；
图2. 保水剂的热稳定性曲线图；
图3. 本发明的改性玉米芯保水剂吸水前的扫描电镜图；
图4. 本发明的改性玉米芯保水剂吸水后的扫描电镜图。
具体实施方式
实施例1
一种可降解玉米芯生物质保水剂的制备方法，其具体制备工艺如下：先用粉碎机将干燥的玉米芯粉碎至200目，称取1000g在100w下微波辐射改性10min，将微波辐射后的玉米芯投入2L 0.5mol/L的乙酸酐溶液中，在60℃下反应4h，然后用水冲洗2-3次，烘干，备用。
称取二次改性后的玉米芯粉末10g分散于150ml水中，在50℃糊化0.5h；然后向体系中加入80g丙烯酰胺，搅拌均匀，在氮气保护下，加入0.12g N,N-亚甲基双丙烯酰胺、0.8g过硫酸铵-亚硫酸氢钠至凝胶生成，最后用95%乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂。
实施例2
一种可降解玉米芯生物质保水剂的制备方法，其具体制备工艺如下：先用粉碎机将干燥的玉米芯粉碎至100目，称取1000g在200w下微波辐射改性5min，将微波辐射后的玉米芯投入4L 1mol/L的甲酸酐溶液中，在30℃下反应10h，然后用水冲洗2-3次，烘干，备用。
称取二次改性后的玉米芯粉末10g分散于200ml水中，在80℃糊化1h；然后向体系中加入50g丙烯酰胺，搅拌均匀，在氮气保护下，加入0.4g N，N-二甲基甲酰胺，0.5g过硫酸铵至凝胶生成，最后用50%乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂。
实施例3
一种可降解玉米芯生物质保水剂的制备方法，其具体制备工艺如下：先用粉碎机将干燥的玉米芯粉碎至500目，称取1000g在100w下微波辐射改性20min，将微波辐射后的玉米芯投入2L 0.8mol/L的邻苯二甲酸酐溶液中，在80℃下反应6h，然后用水冲洗2-3次，烘干，备用。
称取二次改性后的玉米芯粉末10g分散于100ml水中，在65℃糊化0.8h；然后向体系中加入100g丙烯酰胺，搅拌均匀，在氮气保护下，加入0.1g 丙三醇，0.6g过硫酸钾，最后用50%乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂。
实施例4
一种可降解玉米芯生物质保水剂的制备方法，其具体制备工艺如下：先用粉碎机将干燥的玉米芯粉碎至50目，称取1000g在150w下微波辐射改性15min，将微波辐射后的玉米芯投入3L 0.3mol/L的马来酸酐溶液中，在50℃下反应5h，然后用水冲洗2-3次，烘干，备用。
称取二次改性后的玉米芯粉末10g分散于300ml水中，在30℃糊化0.5h；然后向体系中加入60g丙烯酰胺，搅拌均匀，在氮气保护下，加入0.4g 双氧水，0.2g 2-酮戊二酸至凝胶生成至凝胶生成，最后用95%乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂。
Claims (5)
1.一种可降解玉米芯生物质保水剂的制备方法，其特征在于：具体包括如下步骤：
A.改性玉米芯：先用粉碎机将干燥的玉米芯粉碎至5-500目，经微波辐射100-300w改性5-20min，然后酸酐改性：所述酸酐改性是将微波辐射后的玉米芯投入0.1-1mol/L酸酐溶液中，在50-90℃下改性4-10h，然后用水冲洗2-3次，烘干，备用；
B.制备可降解生物质保水剂：将步骤A中二次改性后的玉米芯粉末分散于水中，在30-80℃糊化0.5-1h；然后向该分散体系中加入丙烯酰胺，搅拌均匀，在氮气保护下，加入交联剂、引发剂至凝胶生成，最后用乙醇洗涤，干燥，即得可降解玉米芯生物质保水剂；交联剂为： N,N-亚甲基双丙烯酰胺、丙三醇、双氧水中的任意一种；引发剂为：过硫酸铵、过硫酸铵-亚硫酸氢钠、过硫酸钾、2-酮戊二酸中的任意一种。
2.如权利要求1所述一种可降解玉米芯生物质保水剂的制备方法，其特征在于：所述的酸酐溶液是甲酸酐、乙酸酐、邻苯二甲酸酐、马来酸酐中的任意一种。
3.如权利要求1所述一种可降解玉米芯生物质保水剂的制备方法，其特征在于：改性玉米芯粉末与丙烯酰胺的质量比为：1:5-10。
4.如权利要求1或3所述一种可降解玉米芯生物质保水剂的制备方法，其特征在于：改性玉米芯粉末与交联剂的质量比为：100:0.5-5。
5.如权利要求4所述一种可降解玉米芯生物质保水剂的制备方法，其特征在于：改性玉米芯粉末与引发剂的质量比为：100:1-10。
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