CN110591455A - 一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法 - Google Patents
一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法 Download PDFInfo
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Abstract
本发明涉及一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法,封闭剂由以下按重量百分比计的组分制备而成:虾壳蟹壳分离出的壳聚糖15~20%、纳米二氧化钛溶胶5~7%、聚四氟乙烯1.0~1.5%、1,5,6,7‑四氢环戊并[d]嘧啶‑4‑酮0.4%、2‑氨基‑4‑三氟甲基嘧啶‑5‑羧酸乙酯0.7%、润滑剂0.5%、成膜剂1.0%、表面改性剂0.4%、硅烷偶联剂1.0%,余量为去离子水。该封闭剂干燥后为均一、平整、不变色的透明薄膜,对室内装饰材料及建材家具封闭效果好。附着力强不易脱落安全稳定,耐候性强。且制备过程简单,实用性高。
Description
技术领域
本发明涉及空气净化的技术领域,特别是涉及一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法。
背景技术
甲醛是室内空气主要污染物,甲醛已被世界卫生组织公认为致癌及至畸的物质。长期暴露于甲醛含量超标的空气环境下,会导致眼睛和呼吸道的炎症,慢性过敏性皮炎、色斑,更严重的是,甲醛作为已经明确的一类致癌物,其对室内空气的污染与当今快速增长的癌症、白血病等严重疾 病的患病率密切相关。甲醛主要来源于各种装修装饰材料及建材家具之中,由于其成本低廉制造简单,仍被大量应用。有相关研究表明,甲醛在这些装修装饰材料及建材家具中的释放期一般达到5-15年。因此即使开窗通风几个月至半年,入住后人们仍将长期生活在严重污染环境下,对身体健康造成严重威胁。对于新装修的房子,国内廉价装修装饰材料及建材家具的使用,其中甲醛含量大大超标,严重危害人们的身体健康。必须彻底清除室内甲醛污染物的污染,保护人们身体健康。人们开发了一种有效从源头来阻止甲醛释放的空气净化剂,甲醛封闭剂。考虑抑制甲醛的持续释放,即对污染源进行“封闭”,从源头切断甲醛的释放。封闭剂需要在保证良好的成膜能力的基础上,兼顾交联密度、单体分子量、单体种类、功能性官能团 选择等一系列因素,以确保漆膜在硬度、流平性、粘接强度等参数上取得平衡,更重要的是,对甲醛分子起到屏蔽拦截作用。将其施工在装修装饰材料和建材家具基体表面,干燥后可以形成一层均匀致密透明的封闭膜,从而阻止基体内部甲醛的释放。现有的甲醛封闭剂存在着很多不足,封闭膜耐候性稳定性差,易出现裂缝,附着力差易脱落。
针对于上述问题,亟需开发一种附着力强,不易脱落,封闭效果好,耐候性好,安全稳定的甲醛封闭剂。
发明内容
本发明的目的在于避免现有技术中的不足之处而提供一种密封性强,风力效果好,耐候性稳定,安全环保,有效保证室内环境安全无甲醛的甲醛封闭剂。
本发明的目的通过以下技术方案实现:
提供一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法,其制备原料包括有:
壳聚糖 15~20%、
纳米二氧化钛溶胶 5~7%、
聚四氟乙烯 1.0~1.5%、
1,5,6,7-四氢环戊并[d]嘧啶-4-酮 0.4%、
2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯 0.7%、
聚醚改性烷基共聚物 0.5%、
聚乙烯醇或聚乙烯吡咯烷酮 1.0%、
三异硬脂酰基钛酸异丙酯 0.4%、
硅烷偶联剂 1.0%,
余量为去离子水;
所述壳聚糖由虾壳蟹壳提取获得。
优选的,所述的表硅烷偶联剂为乙烯基三(β-甲氧乙氧基)硅烷、异丁基三乙氧基硅中的一种。
本发明的另一目的在于避免现有技术中的不足之处而提供一种密封性强,风力效果好,耐候性稳定,安全环保,有效保证室内环境安全无甲醛的甲醛封闭剂的制备方法。
本发明的另一目的通过以下技术方案实现
一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法的制备方法包括有以下步骤:
一、制备壳聚糖:
1.1将虾壳蟹壳洗净破碎后置于球磨机中进行研磨,先在3%的稀HCL溶液中浸泡8~12小时后在3%NaOH溶液中浸泡2~4小时,抽滤获得固体,其中每50g虾壳蟹壳粉末配300ml的稀HCL和300ml的NaOH溶液;
1.2步骤(1)获得的固体用100mL浓度为0.02mol/L的KMnO4 溶液浸泡加热脱色(氧化脱虾红素) ,抽滤得固体甲壳素;
1.3烘箱80℃干燥后的甲壳素用45%NaOH溶液脱乙酰基,抽滤得到固体壳聚糖粉末,洗涤后烘干待用;
二、制备甲醛封闭剂
2.1将壳聚糖、纳米二氧化钛溶胶、三异硬脂酰基钛酸异丙酯、硅烷偶联剂和去离子水按照权利要求1的比例投放,高速搅拌时间50~70min,转速为8000~10000转/分,然后超声25~35min,超声后继续高速搅拌20~40min,转速为8000~10000转/分;
2.2往步骤2.1的混合液逐滴加入聚四氟乙烯,缓慢搅拌混合同时加热20~40min,继续加入1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯,快速搅拌混合55~65min,转速为2000转/分;
2.3往步骤2.2的混合体系中加入聚醚改性烷基共聚物、聚乙烯醇或聚乙烯吡咯烷酮,缓慢搅拌8~15min,然后超声8~15min即得到甲醛封闭剂。
本发明的有益效果:
本发明的甲醛封闭剂的制备原料包括有壳聚糖15~20%、纳米二氧化钛溶胶5~7%、聚四氟乙烯1.0~1.5%、1,5,6,7-四氢环戊并[d]嘧啶-4-酮0.4%、2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯0.7%、聚醚改性烷基共聚物0.5%、聚乙烯醇或聚乙烯吡咯烷酮1.0%、三异硬脂酰基钛酸异丙酯0.4%、硅烷偶联剂1.0%,余量为去离子水。其中,本发明的壳聚糖由虾壳蟹壳分离出的壳聚糖改性获得,相对分子质量约为3×105~7×105,粘度高能够有效吸附甲醛并且附着于家具家装表面,对甲醛具有优异的封闭作用。1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯作为填料并对甲醛具有一定的封闭作用。同时,本发明的聚醚改性烷基共聚物、聚乙烯醇或聚乙烯吡咯烷酮可有助于甲醛封闭剂均匀平滑地包裹甲醛并在干燥后形成均匀、平整的透明薄膜将甲醛封闭起来从源头上阻止甲醛的释放。而且,纳米二氧化钛可作为光触媒,装修装饰材料和建材家具释放出的甲醛在紫外光照射下可以被二氧化钛催化分解成二氧化碳和水从根本上解决甲醛污染问题。本发明的封闭剂干燥成膜后,附着力强,密闭性强,封闭效果好,耐候性稳定性好,有效阻止甲醛释放。持续时间长,效率高,安全环保无二次污染。使用简便,只需喷涂装修装饰材料和建材家具基体表面,干燥后可以形成一层均一、平整、不变色的透明薄膜将甲醛封闭起来,从而从源头阻止基材内部甲醛的释放。
具体实施方式
结合以下实施例对本发明作进一步说明。
实施例1
本实施例的一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法的制备原料包括有以下含量的组分:
壳聚糖 15g、
纳米二氧化钛溶胶 5g、
聚四氟乙烯 1.0g、
1,5,6,7-四氢环戊并[d]嘧啶-4-酮 0.4g、
2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯 0.7g、
聚醚改性烷基共聚物 0.5g、
聚乙烯醇或聚乙烯吡咯烷酮 1.0g、
三异硬脂酰基钛酸异丙酯 0.4g、
硅烷偶联剂 1.0g,
去离子水 75g;
其中,所述壳聚糖由虾壳蟹壳提取获得。
所述的表硅烷偶联剂为乙烯基三(β-甲氧乙氧基)硅烷、异丁基三乙氧基硅中的一种。
甲醛封闭剂的制备方法包括有以下步骤:
一、制备壳聚糖:
1.1将虾壳蟹壳洗净破碎后置于球磨机中进行研磨,取50g先300mL在3%的稀HCL溶液中浸泡8小时后在300mL的3%NaOH溶液中浸泡2小时,抽滤获得固体;
1.2步骤(1)获得的固体用100ml 浓度为0.02mol/L的KMnO4 溶液浸泡加热保持在70℃脱色(氧化脱虾红素) ,抽滤得固体甲壳素;
1.3干燥后的甲壳素用45%NaOH溶液脱乙酰基,抽滤得到固体壳聚糖粉末,洗涤后烘干待用;
二、制备甲醛封闭剂
2.1将壳聚糖、纳米二氧化钛溶胶、三异硬脂酰基钛酸异丙酯、硅烷偶联剂和去离子水按比例投放,高速搅拌时间50min,转速为8000~10000转/分,然后超声25min,超声后继续高速搅拌20min,转速为8000~10000转/分;
2.2往步骤2.1的混合液逐滴加入聚四氟乙烯,缓慢搅拌混合同时加热20min,继续加入1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯,快速搅拌混合55min,转速为2000转/分;
2.3往步骤2.2的混合体系中加入聚醚改性烷基共聚物、聚乙烯醇或聚乙烯吡咯烷酮,缓慢搅拌8min,然后超声8min即得到甲醛封闭剂。
实施例2
本实施例的主要技术方案与实施例1基本相同,在本实施例中未作解释的特征,采用实施例1中的解释,在此不再进行赘述。本实施例与实施例1的不同之处在于:
壳聚糖 18%、
纳米二氧化钛溶胶 6%、
聚四氟乙烯 1.2%、
去离子水 70.8g;
其中,所述壳聚糖由虾壳蟹壳提取获得。
甲醛封闭剂的制备方法与实施例1的不同之处在于:
1.1稀HCL溶液中浸泡10小时后在3%NaOH溶液中浸泡3小时;
2.1先高速搅拌时间60min,然后超声30min,超声后继续高速搅拌30min;
2.2往步骤2.1的混合液逐滴加入聚四氟乙烯,缓慢搅拌混合同时加热30min,继续加入1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯,快速搅拌混合60min;
2.3搅拌10min,然后超声10min。
实施例3
本实施例的主要技术方案与实施例1基本相同,在本实施例中未作解释的特征,采用实施例1中的解释,在此不再进行赘述。本实施例与实施例1的不同之处在于:
壳聚糖 20%、
纳米二氧化钛溶胶 7%、
聚四氟乙烯 1.5%、
去离子水 67.5g;
甲醛封闭剂的制备方法与实施例1的不同之处在于:
1.1稀HCL溶液中浸泡12小时后在3%NaOH溶液中浸泡4小时;
2.1先高速搅拌时间70min,然后超声35min,超声后继续高速搅拌40min;
2.2往步骤2.1的混合液逐滴加入聚四氟乙烯,缓慢搅拌混合同时加热35min,继续加入1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯,快速搅拌混合65min;
2.3搅拌15min,然后超声15min。
实施例4
本实施例的主要技术方案与实施例1基本相同,在本实施例中未作解释的特征,采用实施例1中的解释,在此不再进行赘述。本实施例与实施例1的不同之处在于:一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法主要由以下按重量百分比计的组分制备而成:虾壳蟹壳分离出的壳聚糖17g、纳米二氧化钛溶胶6g、聚四氟乙烯1.5g、1,5,6,7-四氢环戊并[d]嘧啶-4-酮0.4g、2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯0.7g、聚醚改性烷基共聚物0.5g、聚乙烯吡咯烷酮1.0g、三异硬脂酰基钛酸异丙酯0.4g、异丁基三乙氧基硅1.0g,余量为去离子水71.5g。
实施例5
本实施例的主要技术方案与实施例1基本相同,在本实施例中未作解释的特征,采用实施例1中的解释,在此不再进行赘述。本实施例与实施例1的不同之处在于:一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法主要由以下按重量百分比计的组分制备而成:虾壳蟹壳分离出的壳聚糖19g、纳米二氧化钛溶胶5.8g、聚四氟乙烯1.2g。
实验测试:
将实施例1至实施例5进行性能测试,测试结果如下:
最后应当说明的是,以上实施例仅用于说明本发明的技术方案说明而非对权利要求保护范围的限制。本领域的普通技术人员参照较佳实施例应当理解,并可以对本发明的技术方案进行修改或者等同替换,但属于本发明技术方案的实质相同和保护范围。
Claims (3)
1.一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法,其特征在于,制备原料包括有:
壳聚糖 15~20%、
纳米二氧化钛溶胶 5~7%、
聚四氟乙烯 1.0~1.5%、
1,5,6,7-四氢环戊并[d]嘧啶-4-酮 0.4%、
2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯 0.7%、
聚醚改性烷基共聚物 0.5%、
聚乙烯醇或聚乙烯吡咯烷酮 1.0%、
三异硬脂酰基钛酸异丙酯 0.4%、
硅烷偶联剂 1.0%,
余量为去离子水;
所述壳聚糖由虾壳蟹壳提取获得。
2.根据权利要求1所述的.一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法,其特征在于,所述的表硅烷偶联剂为乙烯基三(β-甲氧乙氧基)硅烷、异丁基三乙氧基硅中的一种。
3.一种虾壳蟹壳壳聚糖甲醛封闭剂及其制备方法的制备方法,其特征在于,用于制备如权利要求1或2所述的由虾壳蟹壳分离出的壳聚糖改性的甲醛封闭剂,包括有以下步骤:
一、制备壳聚糖:
1.1将虾壳蟹壳洗净破碎后置于球磨机中进行研磨,先在3%的稀HCL溶液中浸泡8~12小时后在3%NaOH溶液中浸泡2~4小时,抽滤获得固体,其中每50g虾壳蟹壳粉末配300ml的稀HCL和300ml的NaOH溶液;
1.2步骤(1)获得的固体用100ml浓度为0.02mol/L的KMnO4 溶液浸泡加热脱色,抽滤得固体甲壳素;
1.3烘箱80℃干燥后的甲壳素用45%NaOH溶液脱乙酰基,抽滤得到固体壳聚糖粉末,洗涤后烘干待用;
二、制备甲醛封闭剂
2.1将壳聚糖、纳米二氧化钛溶胶、三异硬脂酰基钛酸异丙酯、硅烷偶联剂和去离子水按照权利要求1的比例投放,高速搅拌时间50~70min,转速为8000~10000转/分,然后超声25~35min,超声后继续高速搅拌20~40min,转速为8000~10000转/分;
2.2往步骤2.1的混合液逐滴加入聚四氟乙烯,缓慢搅拌混合同时加热70℃20~40min,继续加入1,5,6,7-四氢环戊并[d]嘧啶-4-酮和2-氨基-4-三氟甲基嘧啶-5-羧酸乙酯,快速搅拌混合55~65min,转速为2000转/分;
2.3往步骤2.2的混合体系中加入聚醚改性烷基共聚物、聚乙烯醇或聚乙烯吡咯烷酮,缓慢搅拌8~15min,然后超声8~15min即得到甲醛封闭剂。
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