废弃羊毛、禽毛角蛋白的降解及资源化利用研究
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摘要
在全球资源特别是石油日趋紧缺、环境问题日益严重的今天,有关废弃物的资源化再利胜研究已成为一个引人注意的研究课题。我国制革工业和养殖业规模庞大,每年都产生大量的废弃羊毛、禽毛等固体废弃物,但这些可再生的角蛋白资源目前尚未得到合理利用,大多采用填埋处理,既占用土地,又对大气、水体、士壤等造成严重的污染。同时,以石油为原料的化工产品如皮革合成鞣剂、塑料材料等,由于难以降解对环境产生严重污染,如众所周知的“白色污染”。因此,利用这些弃置会产生危害的角蛋白废弃物——羊毛、禽毛等天然资源制备制革鞣剂和可降解薄膜,以代替基于石油产品的合成鞣剂和塑料薄膜,具有非常重要的科学价值和经济意义及社会效益。
本论文的第一章综述了角蛋白的应用基础、资源状况及国内外研究现状,论述了利用废弃羊毛、禽毛角蛋白资源化利用的前景及应用研究中存在的主要问题,确定了本课题的研究目的、指导思想及研究内容。
第二章研究了超声波处理废弃羊毛制备角蛋白水解液、接枝改性及其在制革中的应用。首次将预处理剂和超声波辐射用于废弃羊毛酸水解制取角蛋白溶液的过程中,有效提高了废弃羊毛的水解效率,大大降低了酸用量,同时显著改善了酸水解羊毛角蛋白分子量的均匀性。将羊毛角蛋白水解液直接应用于铬鞣中,对坯革有明显增厚效果,可提高革的抗张强度和撕裂强度,增加了革的透水汽性,减少鞣制废液中的铬含量。
进而用丙烯酰胺与经过超声辐射处理的角蛋白进行接枝共聚,制备成角蛋白改性产品应用于铬鞣中,改性产品在皮革鞣制中能够替代一半铬鞣剂,能有效减少铬鞣剂用量,而且具有良好的选择填充性,提高了成革的质量。既合理地处理了废弃羊毛,变废为宝,节约资源,又对皮革工业及环境保护有积极意义,为制革少铬鞣制的清洁化生产开辟一条新的途径。第三章研究了废弃羊毛、禽毛制备角蛋白基薄膜的条件和方法。优化了还原法和碱氧化法制取废弃羊毛角蛋白的条件。研究了超声辐照在还原法和碱氧化法制取中的应用,超声可大大缩短水浴加热水解时间,提高碱氧化和还原水解的效率。利用GPC和XRD分析了角蛋白的分子量大小和结构,DSC-TG分析表明所用的水解方法得到的角蛋白有较好的热稳定性。
探索并优化了角蛋白与聚乙烯醇PVA共混制备角蛋白聚乙烯醇复合薄膜的条件,XRD分析表明,薄膜的结构受角蛋白分子质量大小、角蛋白与PVA共混的质量比、共混温度、交联剂和增塑剂的影响。AFM分析表明薄膜表面比较光滑平整,结构致密,角蛋白与PVA有很好的相容性。差示扫描量热分析和热分析表明氧化性角蛋白与还原性角蛋白在高温条件下与PVA共混或通过超声波处理角蛋白,能有效地改善薄膜的热性能。经测定,本文制备的角蛋白薄膜的拉伸强度达到聚乙烯吹塑薄膜国家标准(GB4455-94)一等品(12MPa)或优等品(14MPa)的水平。
薄膜的降解性能实验结果表明,薄膜有很好的自然降解性能；菜籽育种的发芽实验结果表明,薄膜具有较好的保水和保温功能。
第四章研究利用制革废弃羊毛提取胱氨酸,采用预处理的方法缩短了羊毛水解时间,提高胱氨酸的提取率,水解的最优条件是：32%盐酸、酸毛质量比1.8：1、水解温度120℃、水解时间8h。提取的胱氨酸产品含量98.56%。
本论文研制有应用前景的角蛋白鞣剂和角蛋白复合薄膜可丰富角蛋白的应用研究方法,为角蛋白的利用提供理论依据,使废弃羊毛、禽毛这一宝贵的蛋白资源得到合理有效的利用,为角蛋白的深度开发利用和改性制备新型材料提供了新的研究思路和方法。
Nowadays, studies on recycling wastes are gaining increasing attention because of the shortage of resources, particularly petroleum, and the more serious environmental problems. The large scale leather industry and poultry farming in our country produce great quantities of solid wastes each year from waste wool and feather. However, these reproducible keratin resources haven't yet got reasonable exploitation currently, with the most being treated by filling and burying. This result in impropriate land occupation, and brings serious pollution to atmosphere, water and soil environment. Meanwhile, the chemical products which have the petroleum as raw material, such as synthesized tan agent and plastic materials, produce serious environmental pollution that is difficult to degrade, such as the "white pollution" that we all know. Therefore, to reuse these natural resources of wool and feather, which otherwise will produce harm when abandand, in the produce of tanning agent and degradable film to substitute for petroleum-based synthesized tan agent and plastic film is of important scientific value, great economic significance and social benefit.
The applied base, resources condition and studies progress at home and broad of keratin are reviewed in chapter 1.The prospects of recycling waste wool and feather keratin and the main problem in the research are put forward. At the same time, the aim of research, instruction thought and research content are ascertained.
The preparation of keratin hydrolysate from waste wool by ultrasonic, the graft modification and its application in tan leather are illustrated in chapter 2. The use of pretreatment agent and ultrasonic in the preparation keratin by acid hydrolysis of waste wool has not been reported yet. The advantages of this method include:firstly, the hydrolysis rate is enhanced effectively; secondly, the dosage of acid is decreased greatly; thirdly, the molecular weight uniformity of keratin is improved evidently. The use of keratin hydrolysate in chrome tan has obvious incrassation effects on crust, and can raise the tensile strength and tearing strength, increase the water vapor of leather, and reduce the chrome content in the tanning waste.
The application of keratin modification product that is prepared by graft copolymerization of ultrasonic keratin and acrylamide in chrome tan, can replace half chrome tanning agent, reduce the dosage of chrome tanning agent effectively, has good choice filling property and could raise quality of leather. Moreover, it not only treats waste wool reasonably but also has great significance to leather industry and environment protection. This method develops a novel route for the leather industrial cleaning production.
The reaction condition and preparation method of keratin based film from waste wool and feather are explained in chapter 3.The preparation condition of keratin by reduction and alkali oxidization is optimized. The application of ultrasonic in the reaction can shorten hydrolysis time and raise hydrolytic efficiency. The molecular size and structure are analyzed by the GPC and XRD. The result of DSC-TG indicates that the prepared keratin has good thermal stability.
The preparation conditions of composite films from keratin hydrolysate and polyvinyl alcohol (PVA) are explored and optimized. The analysis of XRD shows that the structure of the thin films is affected by keratin molecule size, the mass ratio of keratin and PVA, blend temperature, cross linker and plasticizer. The film has compact structure, smooth and neat surface, and there was good compatibility between keratin and PVA, which can be concluded from the AFM analysis. The result of DSC-TG shows that the blend of PVA and keratin from different methods under high temperature can improve the thermal property of film. The result of measurement displayed that the tensile strengthen of prepared film can reach the China standard (GB4455-94).
The degradation experiments of the film show that the film has good property to naturally degrade. The germination experiment of the rapeseed shows the films have good properties to protect the water and preserve heat functions.
The technology of extracting cystine from the waste wool that was from leather making industry is studied in chapter 4. The optimum condition for the hydrolysis is the mixture of acid and wool in a mass ratio of 1.8:1,120℃temperature and 8h for reaction.The content of cystine is 98.56%.
The development of keratin tanning agent and keratin composite film, which has potential application foreground, provides the theoretical basis for the exploitation of keratin, makes these precious keratin resources of wool and feather going to reasonable utilization, and offer new ideals and a new approach to the exploitation of keratin and modified preparation novel materials.
本论文的第一章综述了角蛋白的应用基础、资源状况及国内外研究现状,论述了利用废弃羊毛、禽毛角蛋白资源化利用的前景及应用研究中存在的主要问题,确定了本课题的研究目的、指导思想及研究内容。
第二章研究了超声波处理废弃羊毛制备角蛋白水解液、接枝改性及其在制革中的应用。首次将预处理剂和超声波辐射用于废弃羊毛酸水解制取角蛋白溶液的过程中,有效提高了废弃羊毛的水解效率,大大降低了酸用量,同时显著改善了酸水解羊毛角蛋白分子量的均匀性。将羊毛角蛋白水解液直接应用于铬鞣中,对坯革有明显增厚效果,可提高革的抗张强度和撕裂强度,增加了革的透水汽性,减少鞣制废液中的铬含量。
进而用丙烯酰胺与经过超声辐射处理的角蛋白进行接枝共聚,制备成角蛋白改性产品应用于铬鞣中,改性产品在皮革鞣制中能够替代一半铬鞣剂,能有效减少铬鞣剂用量,而且具有良好的选择填充性,提高了成革的质量。既合理地处理了废弃羊毛,变废为宝,节约资源,又对皮革工业及环境保护有积极意义,为制革少铬鞣制的清洁化生产开辟一条新的途径。第三章研究了废弃羊毛、禽毛制备角蛋白基薄膜的条件和方法。优化了还原法和碱氧化法制取废弃羊毛角蛋白的条件。研究了超声辐照在还原法和碱氧化法制取中的应用,超声可大大缩短水浴加热水解时间,提高碱氧化和还原水解的效率。利用GPC和XRD分析了角蛋白的分子量大小和结构,DSC-TG分析表明所用的水解方法得到的角蛋白有较好的热稳定性。
探索并优化了角蛋白与聚乙烯醇PVA共混制备角蛋白聚乙烯醇复合薄膜的条件,XRD分析表明,薄膜的结构受角蛋白分子质量大小、角蛋白与PVA共混的质量比、共混温度、交联剂和增塑剂的影响。AFM分析表明薄膜表面比较光滑平整,结构致密,角蛋白与PVA有很好的相容性。差示扫描量热分析和热分析表明氧化性角蛋白与还原性角蛋白在高温条件下与PVA共混或通过超声波处理角蛋白,能有效地改善薄膜的热性能。经测定,本文制备的角蛋白薄膜的拉伸强度达到聚乙烯吹塑薄膜国家标准(GB4455-94)一等品(12MPa)或优等品(14MPa)的水平。
薄膜的降解性能实验结果表明,薄膜有很好的自然降解性能；菜籽育种的发芽实验结果表明,薄膜具有较好的保水和保温功能。
第四章研究利用制革废弃羊毛提取胱氨酸,采用预处理的方法缩短了羊毛水解时间,提高胱氨酸的提取率,水解的最优条件是：32%盐酸、酸毛质量比1.8：1、水解温度120℃、水解时间8h。提取的胱氨酸产品含量98.56%。
本论文研制有应用前景的角蛋白鞣剂和角蛋白复合薄膜可丰富角蛋白的应用研究方法,为角蛋白的利用提供理论依据,使废弃羊毛、禽毛这一宝贵的蛋白资源得到合理有效的利用,为角蛋白的深度开发利用和改性制备新型材料提供了新的研究思路和方法。
Nowadays, studies on recycling wastes are gaining increasing attention because of the shortage of resources, particularly petroleum, and the more serious environmental problems. The large scale leather industry and poultry farming in our country produce great quantities of solid wastes each year from waste wool and feather. However, these reproducible keratin resources haven't yet got reasonable exploitation currently, with the most being treated by filling and burying. This result in impropriate land occupation, and brings serious pollution to atmosphere, water and soil environment. Meanwhile, the chemical products which have the petroleum as raw material, such as synthesized tan agent and plastic materials, produce serious environmental pollution that is difficult to degrade, such as the "white pollution" that we all know. Therefore, to reuse these natural resources of wool and feather, which otherwise will produce harm when abandand, in the produce of tanning agent and degradable film to substitute for petroleum-based synthesized tan agent and plastic film is of important scientific value, great economic significance and social benefit.
The applied base, resources condition and studies progress at home and broad of keratin are reviewed in chapter 1.The prospects of recycling waste wool and feather keratin and the main problem in the research are put forward. At the same time, the aim of research, instruction thought and research content are ascertained.
The preparation of keratin hydrolysate from waste wool by ultrasonic, the graft modification and its application in tan leather are illustrated in chapter 2. The use of pretreatment agent and ultrasonic in the preparation keratin by acid hydrolysis of waste wool has not been reported yet. The advantages of this method include:firstly, the hydrolysis rate is enhanced effectively; secondly, the dosage of acid is decreased greatly; thirdly, the molecular weight uniformity of keratin is improved evidently. The use of keratin hydrolysate in chrome tan has obvious incrassation effects on crust, and can raise the tensile strength and tearing strength, increase the water vapor of leather, and reduce the chrome content in the tanning waste.
The application of keratin modification product that is prepared by graft copolymerization of ultrasonic keratin and acrylamide in chrome tan, can replace half chrome tanning agent, reduce the dosage of chrome tanning agent effectively, has good choice filling property and could raise quality of leather. Moreover, it not only treats waste wool reasonably but also has great significance to leather industry and environment protection. This method develops a novel route for the leather industrial cleaning production.
The reaction condition and preparation method of keratin based film from waste wool and feather are explained in chapter 3.The preparation condition of keratin by reduction and alkali oxidization is optimized. The application of ultrasonic in the reaction can shorten hydrolysis time and raise hydrolytic efficiency. The molecular size and structure are analyzed by the GPC and XRD. The result of DSC-TG indicates that the prepared keratin has good thermal stability.
The preparation conditions of composite films from keratin hydrolysate and polyvinyl alcohol (PVA) are explored and optimized. The analysis of XRD shows that the structure of the thin films is affected by keratin molecule size, the mass ratio of keratin and PVA, blend temperature, cross linker and plasticizer. The film has compact structure, smooth and neat surface, and there was good compatibility between keratin and PVA, which can be concluded from the AFM analysis. The result of DSC-TG shows that the blend of PVA and keratin from different methods under high temperature can improve the thermal property of film. The result of measurement displayed that the tensile strengthen of prepared film can reach the China standard (GB4455-94).
The degradation experiments of the film show that the film has good property to naturally degrade. The germination experiment of the rapeseed shows the films have good properties to protect the water and preserve heat functions.
The technology of extracting cystine from the waste wool that was from leather making industry is studied in chapter 4. The optimum condition for the hydrolysis is the mixture of acid and wool in a mass ratio of 1.8:1,120℃temperature and 8h for reaction.The content of cystine is 98.56%.
The development of keratin tanning agent and keratin composite film, which has potential application foreground, provides the theoretical basis for the exploitation of keratin, makes these precious keratin resources of wool and feather going to reasonable utilization, and offer new ideals and a new approach to the exploitation of keratin and modified preparation novel materials.
引文
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