CN115322267B - 一种生物质基两性合成鞣剂的制备方法 - Google Patents
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Abstract
本发明公开了一种生物质基两性合成鞣剂的制备方法。具体制备方法如下:保持温度为0~5 oC,以氨基多糖为反应底物,在水溶液中与三聚氯氰发生亲核取代反应,控制氨基多糖与三聚氯氰的质量比在一定范围,反应5~10 h,即得到浅黄色生物质基两性合成鞣剂。本发明方法制备的生物质基两性合成鞣剂结构中含有多个碳氯键、羟基、氨基等活性基团,具有良好的水溶性、鞣制性能及填充性,鞣革色浅、具有较好的耐湿热稳定性、感官性能和物理性能,且可有效革规避皮革中六价铬及游离甲醛带来的环境问题与健康风险。
Description
技术领域
本发明涉及一种生物质基两性合成鞣剂的制备方法,具体属于清洁化皮革鞣剂合成技术领域。
背景技术
现代制革工业的快速发展始于一浴铬鞣法的发明,距今已有上百年的历史。传统铬鞣法鞣革具有收缩温度高,耐水洗能力强,柔软、丰满、弹性和延伸性好等优点,因此在现代制革行业中一直占据主导地位。但与此同时,制革过程中会产生大量的含铬废液,其中Cr(Ⅲ)的含量高达2000-8000 mg/L,经目前广泛采用的碱沉淀法回收处理后,Cr(Ⅲ)的含量仍达不到我国的排放标准(GB 30486-2013)1.5 mg/L,给环境保护及生态平衡造成巨大威胁。此外,研究表明,鞣革使用的Cr(Ⅲ) 在加热、紫外线照射和高pH值等条件下易被氧化为具有强致癌作用的 Cr(Ⅵ),即使是低含量的Cr(Ⅵ) 也能对人的皮肤和呼吸道分别产生过敏性接触性皮炎和强烈的刺激作用,因此国内外对皮革中Cr(Ⅵ) 的含量有相当严格的限制,国内对皮革中Cr(Ⅵ) 限量为5 mg/kg,欧盟更是将该值限制在3 mg/kg。皮革行业也因此面临越来越大的压力。
为解决铬鞣革中六价铬对环境以及人体健康带来的风险问题,预防Cr(Ⅵ)的产生以及发展无铬鞣技术是目前主要的研究方向。国内外对于皮革中Cr(Ⅵ)的预防措施主要有栲胶复鞣,使用加脂助剂,添加抗氧化剂等,但这些措施仍无法从根本上消除六价铬的危害。因此从现阶段来看,无铬鞣替代技术被认为是最佳选择。
现有的无铬鞣法主要包括非铬金属鞣、植鞣、醛鞣、有机磷鞣等。非铬金属鞣主要采用Al(Ⅲ)、Zr(Ⅳ) 及Ti(Ⅳ) 进行鞣制,但往往存在以下缺点:Al(Ⅲ) 鞣革收缩温度较低(75~85℃),不耐水洗,Zr(Ⅳ) 鞣革过于紧实板硬,且成本较高,Ti(Ⅳ)在鞣制过程中存在极易水解沉淀,在皮胶原内分布不均等问题,因而目前还无法完全替代铬鞣;植鞣革成革紧实、丰满有弹性、卫生性能及可生物降解性良好,但由于植物鞣剂与胶原纤维间无牢固化学键结合,遇水易脱鞣,因此纯植鞣革的收缩温度通常无法满足成革的要求,且植物鞣剂本身具有一定的颜色,故坯革颜色较深,不利于后期染色;醛鞣革成革色浅,粒面细致,手感柔软丰满,具有耐水洗、耐汗、耐氧化等突出优点,但醛鞣革不耐黄变,故不适用于浅色革的生产,且存在甲醛超标的风险,制约了醛鞣法的发展;有机磷鞣革色泽洁白、耐黄变、抗撕裂性能优良,且成革具有良好的阻燃性,但收缩温度较低(80~85 oC),且在鞣制过程中存在游离甲醛释放的问题,对接触者的身体健康造成巨大威胁,因而其应用也受到限制。
总之,目前主要的无铬鞣技术所得成革还无法完全满足行业及市场的需求,同时给环境以及人体健康带来的危害也无法忽视。因此,本发明的目的是提供一种鞣性良好、绿色环保且无害的新型鞣剂。
发明内容
本发明提供一种生物质基两性合成鞣剂的制备方法。为达到上述目的,本发明采用以下技术方案来实现,具体操作方法如下:
准确称取一定量三聚氯氰置于三口烧瓶中并加入适量的去离子水,在机械搅拌作用下使三聚氯氰在水中充分分散;控制内温为0~5 oC,逐滴滴加浓度为40% w/v的氨基多糖水溶液,控制三聚氯氰和氨基多糖的质量比为(0.05~0.6):1,并同时滴加浓度为5%~10% w/v的碱溶液以调节反应pH为3.0~8.0,搅拌反应5~10 h后,将反应体系抽滤两次,滤液经过冷冻干燥,研磨得到浅黄色固体粉末,即为所合成的生物质基两性合成鞣剂,其化学结构式如下:
(R为氨基多糖)。
本发明所述的一种生物质基两性合成鞣剂的制备方法,其特征在于所述的氨基多糖为壳寡糖、透明质酸、硫酸软骨素中的一种。
本发明所述的一种生物质基两性合成鞣剂的制备方法,其特征在于所述的生物质基两性合成鞣剂的分子量在500~5000范围内,且具有多分散性,因而在鞣制过程中能够渗透进入胶原各层级结构,促进鞣剂在胶原分子上的结合。
本发明所述的一种生物质基两性合成鞣剂的制备方法,其特征在于所述的生物质基两性合成鞣剂结构中含有多个碳氯键、羟基、氨基等活性基团,具有良好的水溶性及鞣制性能,可赋予皮革良好的耐湿热稳定性及物理性能。
本发明所述的一种生物质基两性合成鞣剂的制备方法,其特征在于所述的生物质基两性合成鞣剂结构中含有多个的氨基及羟基,为两性物质,在染色、加脂等后序工艺中通过调整体系pH可促进酸性染料、阴离子型加脂剂等阴离子材料的吸收。
本发明所述的一种改性生物质基活性鞣剂的制备方法,具有以下优点:
1)本发明采用氨基多糖为改性原料,由可再生生物质资源水解得到,来源广泛,具有良好的水溶性、生物相容性及可生物降解性;
2)本发明采用三聚氯氰与氨基多糖作为反应物,水作为该反应体系的分散相,合成及鞣制过程中都不会有六价铬、甲醛等有害物质生成,有效规避了皮革中六价铬及游离甲醛带来的健康问题与环境风险;
3)本发明方法制备的生物质基两性合成鞣剂分子中含有多个碳氯键、羟基等活性基团,具有良好的鞣制性能,鞣后坯革增厚明显、赋予坯革良好的耐湿热稳定性其他物理性能。
附图说明
图1为实施例1中三聚氯氰、壳寡糖、改性壳寡糖的红外谱图对照图。
图2为实施例1中三聚氯氰、壳寡糖、改性壳寡糖的核磁共振碳谱图对照图。
具体实施方式
实施例1
称取12.00 g三聚氯氰搅拌分散于装有30 mL去离子水的250 mL三口烧瓶中,称取30.00 g壳寡糖溶解于75 ml去离子水中;保持温度为2 oC,在机械搅拌的作用下,向烧瓶内逐滴滴加壳寡糖水溶液,并在反应过程中不断滴加质量浓度为5%的碳酸钠溶液以控制反应pH为6.0,搅拌反应10 h;反应结束后,将反应体系抽滤两次,滤液经过冷冻干燥,研磨得到浅黄色固体粉末,即为所合成的生物质基两性合成鞣剂。
实施例2
称取5.00 g三聚氯氰搅拌分散于装有30 mL去离子水的250 mL三口烧瓶中,称取10.00 g壳寡糖溶解于25 ml去离子水中;保持温度为2 oC,在机械搅拌的作用下,向烧瓶内逐滴滴加壳寡糖水溶液,并在反应过程中不断滴加质量浓度为5%的碳酸钠溶液以控制反应pH为6.0,搅拌反应10 h;反应结束后,将反应体系抽滤两次,滤液经过冷冻干燥,研磨得到浅黄色固体粉末,即为所合成的生物质基两性合成鞣剂。
实施例3
称取30.00 g三聚氯氰搅拌分散于装有100 ml去离子水的500 ml三口烧瓶中,称取60.00 g壳寡糖溶解于150 ml去离子水中;保持温度为2 oC,在机械搅拌的作用下,向烧瓶内逐滴滴加壳寡糖水溶液,并在反应过程中不断滴加质量浓度为5%的碳酸钠溶液以控制反应pH为5.0,搅拌反应10 h;反应结束后,将反应体系抽滤两次,滤液经过冷冻干燥,研磨得到浅黄色固体粉末,即为所合成的生物质基两性合成鞣剂。
Claims (2)
1.一种生物质基两性合成鞣剂的制备方法,其特征在于具体制备步骤如下:
准确称取一定量三聚氯氰置于三口烧瓶中并加入适量的去离子水,在机械搅拌作用下使三聚氯氰在水中充分分散;控制内温为0~5℃,逐滴滴加浓度为40% w/v的氨基多糖水溶液,控制三聚氯氰和氨基多糖的质量比为(0.05~0.6):1,并同时滴加浓度为5%~10% w/v的碱溶液以调节反应pH为3.0~8.0,搅拌反应5~10 h后,将反应体系抽滤两次,滤液经过冷冻干燥,研磨得到浅黄色固体粉末,即为所合成的生物质基两性合成鞣剂,其化学结构式如下:
;R为壳寡糖,所述氨基多糖为壳寡糖。
2.根据权利要求1所述的一种生物质基两性合成鞣剂的制备方法,其特征在于所述的生物质基两性合成鞣剂的分子量在500~5000范围内,且具有多分散性。
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