CN108219986A - 一种高效果蔬农药清洗剂的制备方法 - Google Patents
一种高效果蔬农药清洗剂的制备方法 Download PDFInfo
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- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D11/04—Special methods for preparing compositions containing mixtures of detergents by chemical means, e.g. by sulfonating in the presence of other compounding ingredients followed by neutralising
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Abstract
本发明涉及一种高效果蔬农药清洗剂的制备方法,属于清洗剂制备技术领域。本发明首先用原硅酸作为硅源,之后加入碱和铝源偏铝酸锂,利用水热法合成硅铝分子筛载体,利用硼化镍作催化剂,通过酒石酸的螯合性能使得硅铝分子筛中的金属离子离开原有的晶格进入酒石酸有机相中,从而在硅铝分子筛的原有晶格上产生空穴,提高分子筛的吸附活性,接着以富含茶皂素的茶籽和富含多糖的螺旋藻作为原料,经水提醇沉的作用,使得茶皂素和螺旋藻多糖析出并被高吸附性的分子筛吸附固着,继续和硝酸铈溶液反应,得到反应滤渣,然后本发明将牡蛎壳粉碎后煅烧,并和水反应,过滤得到碱性的钙离子溶液,最后将钙离子溶液和反应滤渣共混浓缩制得果蔬农药清洗剂。
Description
技术领域
本发明涉及一种高效果蔬农药清洗剂的制备方法,属于清洗剂制备技术领域。
背景技术
由于农药的大量使用,我国水果、蔬菜农药残留超标问题越来越严重。市场上的一些瓜果蔬菜在种植过程中,由于用的农药过多,或者采摘时间离施药时间的间隔过近,在它们表面残留有大量的农药及其代谢物、降解物以及有毒杂质等物质残存,有的甚至侵入了果蔬内部,不易被清水洗掉。人体若长期食用这些被农药污染的瓜果蔬菜, 必会造成有害物质在体内积聚,给人体健康带来潜在威胁,重者还会出现食物中毒,危及生命。特别是有机磷农药对人与动物的毒性作用比较大,有机磷农药经过皮肤、呼吸以及肠胃吸收等途径进入人体后, 对体内胆碱酯酶的活性产生抑制作用, 能阻断神经递质的传递。近年, 全国因误食有残留农药的果蔬中毒案件屡屡发生,经常见诸媒体。食品安全问题一直是人们关注的焦点。
目前去除果蔬农药残留的方法主要有普通的物理方法如焯水、去皮、盐水、碱水清洗等,或者采用化学合成洗涤剂以及臭氧、过碳酸钠降解法、酶降解法等化学方法进行清洗,但它们的农药去除率一般或影响到蔬果营养成分,加上清洗剂中所使用的人工合成化合物如防腐剂、香精、增稠剂等造成果蔬的二次污染,甚至清洗剂自身难以降解进而污染环境等缺陷使得人们更倾向于选择天然环保的果蔬清洗剂。
因此,发明一种对果蔬残留农药去除率高,且不会影响果蔬品质,对人体和环境没有危害的果蔬清洗剂对清洗剂制备技术领域具有积极的意义。
发明内容
本发明主要解决的技术问题,针对目前去除果蔬农药残留的方法对农药去除率一般或影响到蔬果营养成分,所用清洗剂中含有大量人工合成化合物造成果蔬的二次污染,甚至清洗剂自身难以降解进而污染环境的缺陷,提供了一种高效果蔬农药清洗剂的制备方法。
为了解决上述技术问题,本发明所采用的技术方案是:
一种高效果蔬农药清洗剂的制备方法,其特征在于具体制备步骤为:
(1)量取原硅酸溶液,将原硅酸溶液加热升温至100~105℃,搅拌反应1~2h,得到悬浊液,将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;
(2)将上述前驱液移入高压水热釜中,再向高压水热釜中加入硼化镍和浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,水热反应28~30h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;
(3)按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水混合后装入烧杯中,加热升温至60~70℃,用磁力搅拌器保温搅拌浸提3~5h,浸提结束后过滤分离得到滤液;
(4)将上述滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至75~85℃,保温静置陈化3~5h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液混合后在温度为90~95℃的条件下搅拌反应1~3h,反应结束后过滤得到反应滤渣,备用;
(5)称取牡蛎壳放入球磨机中研磨粉碎20~30min,再将研磨粉碎后的牡蛎壳放入高温炉中,保温煅烧2~3h,将煅烧产物和水混合后搅拌反应20~30min,过滤分离得到反应滤液;
(6)按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在70~80℃下旋蒸浓缩30~40min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
步骤(1)中所述的原硅酸溶液的质量分数为60%,悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液的质量比为1:2:10。
步骤(2)中所述的硼化镍的加入量为前驱液质量的2%,浓度为0.5mol/L酒石酸溶液的加入量为前驱液质量的5%,水热反应的压力为1.6~1.7MPa,水热反应的温度为200~210℃。
步骤(3)中所述的粉碎物和水的质量比为1:5。
步骤(4)中所述的滤饼和质量分数为0.05%的硝酸铈溶液的质量比为1:5。
步骤(5)中所述的保温煅烧的温度为900~1000℃,煅烧产物和水的质量比为1:3。
本发明的有益效果是:
本发明首先用原硅酸作为硅源,之后加入碱和铝源偏铝酸锂,利用水热法合成硅铝分子筛载体,在水热反应的过程中加入了硼化镍和酒石酸,利用硼化镍作催化剂,通过酒石酸的螯合性能使得硅铝分子筛中的金属离子离开原有的晶格进入酒石酸有机相中,从而在硅铝分子筛的原有晶格上产生空穴,提高分子筛的吸附活性,得到高吸附性的分子筛作为功能性吸附料,接着以富含茶皂素的茶籽和富含多糖的螺旋藻作为原料,经水提醇沉的作用,使得茶皂素和螺旋藻多糖析出并被高吸附性的分子筛吸附固着,继续和硝酸铈溶液反应,硝酸铈和多糖反应生成多糖稀土配合物负载在分子筛内部孔隙中,过滤得到反应滤渣,然后本发明将牡蛎壳粉碎后煅烧,并和水反应,过滤得到碱性的钙离子溶液,最后将钙离子溶液和反应滤渣共混浓缩制得果蔬农药清洗剂,本发明的果蔬清洗剂使用时,分子筛的高吸附活性使其向果蔬表面靠近,吸附在果树表面,接着分子筛中天然表面活性剂茶皂素最先溶出,作用于果蔬表面的农药,通过表面活性剂改变两者接触面的表面张力使得农药和果蔬产生初步分离,此时负载在分子筛内部孔隙中的多糖稀土配合物与碱性钙离子溶液发生作用,在稀土离子和碱性溶液中氢氧根离子的双重催化作用下,稀土离子和氢氧根离子有选择的进攻磷原子,伴以P-O(S)键的断开,有机磷农药不断水解,水解后的产物再次被分子筛吸附固着,最后在水流的冲刷作用下随着分子筛一起流失,即可完成对果蔬表面残留农药的冲洗,并且本发明的果蔬农药清洗剂原材料大多为天然物质,生物降解性好,无毒无害,不会对人体和环境产生危害,农药去除率高,具有广阔的应用前景。
具体实施方式
量取质量分数为60%的原硅酸溶液,将原硅酸溶液加热升温至100~105℃,继续搅拌反应1~2h,得到悬浊液,按质量比为1:2:10将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;将前驱液移入高压水热釜中,再向高压水热釜中加入前驱液质量2%的硼化镍和前驱液质量5%的浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,在1.6~1.7MPa下加热升温至200~210℃,水热反应28~30h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水按质量比为1:5混合后装入烧杯中,加热升温至60~70℃,用磁力搅拌器保温搅拌浸提3~5h,浸提结束后过滤分离得到滤液;按质量比为2:1:2将滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至75~85℃,保温静置陈化3~5h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液按质量比为1:5混合后在温度为90~95℃的条件下搅拌反应1~3h,反应结束后过滤得到反应滤渣,备用;称取牡蛎壳放入球磨机中研磨粉碎20~30min,再将研磨粉碎后的牡蛎壳放入高温炉中,在900~1000℃下保温煅烧2~3h,将煅烧产物和水按质量比为1:3混合后搅拌反应20~30min,过滤分离得到反应滤液;按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在70~80℃下旋蒸浓缩30~40min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
实例1
量取质量分数为60%的原硅酸溶液,将原硅酸溶液加热升温至100℃,继续搅拌反应1h,得到悬浊液,按质量比为1:2:10将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;将前驱液移入高压水热釜中,再向高压水热釜中加入前驱液质量2%的硼化镍和前驱液质量5%的浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,在1.6MPa下加热升温至200℃,水热反应28h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水按质量比为1:5混合后装入烧杯中,加热升温至60℃,用磁力搅拌器保温搅拌浸提3h,浸提结束后过滤分离得到滤液;按质量比为2:1:2将滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至75℃,保温静置陈化3h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液按质量比为1:5混合后在温度为90℃的条件下搅拌反应1h,反应结束后过滤得到反应滤渣,备用;称取牡蛎壳放入球磨机中研磨粉碎20min,再将研磨粉碎后的牡蛎壳放入高温炉中,在900℃下保温煅烧2h,将煅烧产物和水按质量比为1:3混合后搅拌反应20min,过滤分离得到反应滤液;按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在70℃下旋蒸浓缩30min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
实例2
量取质量分数为60%的原硅酸溶液,将原硅酸溶液加热升温至103℃,继续搅拌反应1h,得到悬浊液,按质量比为1:2:10将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;将前驱液移入高压水热釜中,再向高压水热釜中加入前驱液质量2%的硼化镍和前驱液质量5%的浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,在1.6MPa下加热升温至205℃,水热反应29h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水按质量比为1:5混合后装入烧杯中,加热升温至65℃,用磁力搅拌器保温搅拌浸提4h,浸提结束后过滤分离得到滤液;按质量比为2:1:2将滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至80℃,保温静置陈化4h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液按质量比为1:5混合后在温度为93℃的条件下搅拌反应2h,反应结束后过滤得到反应滤渣,备用;称取牡蛎壳放入球磨机中研磨粉碎25min,再将研磨粉碎后的牡蛎壳放入高温炉中,在950℃下保温煅烧2h,将煅烧产物和水按质量比为1:3混合后搅拌反应25min,过滤分离得到反应滤液;按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在75℃下旋蒸浓缩35min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
实例3
量取质量分数为60%的原硅酸溶液,将原硅酸溶液加热升温至105℃,继续搅拌反应2h,得到悬浊液,按质量比为1:2:10将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;将前驱液移入高压水热釜中,再向高压水热釜中加入前驱液质量2%的硼化镍和前驱液质量5%的浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,在1.7MPa下加热升温至210℃,水热反应30h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水按质量比为1:5混合后装入烧杯中,加热升温至70℃,用磁力搅拌器保温搅拌浸提5h,浸提结束后过滤分离得到滤液;按质量比为2:1:2将滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至85℃,保温静置陈化5h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液按质量比为1:5混合后在温度为95℃的条件下搅拌反应3h,反应结束后过滤得到反应滤渣,备用;称取牡蛎壳放入球磨机中研磨粉碎30min,再将研磨粉碎后的牡蛎壳放入高温炉中,在1000℃下保温煅烧3h,将煅烧产物和水按质量比为1:3混合后搅拌反应30min,过滤分离得到反应滤液;按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在80℃下旋蒸浓缩40min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
对照例
以黑龙江某公司生产的果蔬清洗剂作为对照例
对本发明制得的果蔬清洗剂和对照例中的果蔬清洗剂进行性能检测,检测结果如表1所示:
表1
由上表中检测数据可以看出,本发明制得的果蔬农药清洗剂对果蔬表面农药的去除率高,对环境和人体没有危害,使用前景广阔。
Claims (6)
1.一种高效果蔬农药清洗剂的制备方法,其特征在于具体制备步骤为:
(1)量取原硅酸溶液,将原硅酸溶液加热升温至100~105℃,搅拌反应1~2h,得到悬浊液,将悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液混合得到前驱液;
(2)将上述前驱液移入高压水热釜中,再向高压水热釜中加入硼化镍和浓度为0.5mol/L酒石酸溶液,密闭高压水热釜,水热反应28~30h,待水热反应结束后过滤分离得到滤渣,即为功能性吸附料,备用;
(3)按等质量比将茶籽和螺旋藻混合后用组织粉碎机研磨粉碎,得到粉碎物,将粉碎物和水混合后装入烧杯中,加热升温至60~70℃,用磁力搅拌器保温搅拌浸提3~5h,浸提结束后过滤分离得到滤液;
(4)将上述滤液和备用的功能性吸附料以及质量分数为90%的乙醇溶液混合,移入水浴锅中,加热升温至75~85℃,保温静置陈化3~5h,陈化结束后过滤分离得到滤饼,将滤饼和质量分数为0.05%的硝酸铈溶液混合后在温度为90~95℃的条件下搅拌反应1~3h,反应结束后过滤得到反应滤渣,备用;
(5)称取牡蛎壳放入球磨机中研磨粉碎20~30min,再将研磨粉碎后的牡蛎壳放入高温炉中,保温煅烧2~3h,将煅烧产物和水混合后搅拌反应20~30min,过滤分离得到反应滤液;
(6)按重量比为1:5将备用的反应滤渣和上述反应滤液混合后装入旋转蒸发仪中,在70~80℃下旋蒸浓缩30~40min,得到浓缩液,将浓缩液装罐后即得高效果蔬农药清洗剂。
2.根据权利要求1所述的一种高效果蔬农药清洗剂的制备方法,其特征在于:步骤(1)中所述的原硅酸溶液的质量分数为60%,悬浊液、质量分数为10%氢氧化钠溶液和质量分数为25%的偏铝酸钾溶液的质量比为1:2:10。
3.根据权利要求1所述的一种高效果蔬农药清洗剂的制备方法,其特征在于:步骤(2)中所述的硼化镍的加入量为前驱液质量的2%,浓度为0.5mol/L酒石酸溶液的加入量为前驱液质量的5%,水热反应的压力为1.6~1.7MPa,水热反应的温度为200~210℃。
4.根据权利要求1所述的一种高效果蔬农药清洗剂的制备方法,其特征在于:步骤(3)中所述的粉碎物和水的质量比为1:5。
5.根据权利要求1所述的一种高效果蔬农药清洗剂的制备方法,其特征在于:步骤(4)中所述的滤饼和质量分数为0.05%的硝酸铈溶液的质量比为1:5。
6.根据权利要求1所述的一种高效果蔬农药清洗剂的制备方法,其特征在于:步骤(5)中所述的保温煅烧的温度为900~1000℃,煅烧产物和水的质量比为1:3。
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