羧甲基沙蒿胶的制备、性质及应用
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摘要
本论文主要研究了以沙蒿胶为原料,氯乙酸为醚化剂,在碱性条件下合成羧甲基沙蒿胶的工艺,并研究了羧甲基沙蒿胶的性质、结构及其在速冻水饺中的应用。
通过单因素实验分别研究了碱化反应阶段的碱化时间、碱化温度、沙蒿胶的质量浓度、NaOH与沙蒿胶的摩尔比和醚化反应阶段的醚化时间、醚化温度、乙醇的体积分数、氯乙酸与沙蒿胶的摩尔比、NaOH与沙蒿胶的摩尔比对取代度和反应效率的影响,在此基础上,通过正交实验确定了制备羧甲基沙蒿胶的最佳工艺条件。实验结果表明,碱化反应阶段的最佳工艺条件为:碱化时间为1.5h,碱化温度为35℃,沙蒿胶的质量浓度为40g/L(以沙蒿胶的干基计算),NaOH与沙蒿胶的摩尔比为1∶1;醚化反应阶段的最佳工艺条件为:醚化时间为3h,醚化温度为60℃,乙醇的体积分数为75%,氯乙酸与沙蒿胶的摩尔比为0.6∶1,NaOH与沙蒿胶的摩尔比为0.7∶1。在最优的工艺条件下,得到的羧甲基沙蒿胶的取代度为0.4982,反应效率为83.03%。
对羧甲基沙蒿胶的性质进行了分析,结果表明:通过羧甲基化,当羧甲基沙蒿胶的取代度为0.4982时,其水不溶物含量由原来的56.02%降为15.01%,吸水率由原来的13.02%上升到160.68%;羧甲基沙蒿胶溶液的粘度随着剪切速率的增加而降低,属于非牛顿流体,其表观粘度随着羧甲基沙蒿胶质量分数的增加而增加,温度对羧甲基沙蒿胶粘度的影响随着取代度的增加而呈明显的下降趋势,羧甲基沙蒿胶溶液的粘度随着pH的增加先升高后降低,NaCl会降低羧甲基沙蒿胶溶液的粘度而蔗糖使其粘度升高。另外,通过红外光谱实验得出,改性后的沙蒿胶分别在1730cm~(-1)、1382cm~(-1)和1254cm~(-1)处出现了很强的吸收峰,表明改性后体系中含有-C=O、-CH2和-C-O,因此从原沙蒿胶与改性后的羧甲基沙蒿胶在红外光谱图上的区别可以得出羧甲基已经成功地接到了沙蒿胶上。
将羧甲基沙蒿胶应用于速冻水饺,通过实验确定了较佳的工艺条件,将羧甲基沙蒿胶应用于饺子馅的工艺条件为:取代度为0.4982,添加量为馅料质量的0.2%,冻裂率下降17.14%;将羧甲基沙蒿胶应用于饺子皮的工艺条件为:取代度为0.4982,添加量为面粉质量的0.2%～0.25%,冻裂率下降42.85%。
It was studied in this thesis the preparation of Artemisia glue, under the condition of alkali, chloroacetic acid was used as etherification agent and the properties, structures and application in quick-frozen dumpling were researched too.
In the single factor experiments, the affects of degree of substitution(DS) and reaction efficiency(RE) by some factors,which included,the alkalifying time,the alkalifying temperature,the concentration of Artemisia glue,the mol ratio of NaOH and Artemisia glue (alkalified reaction phase),the etherification time,the etherification temperature,the volume fraction of alcohol,the mol ratio of chloroacetic acid and Artemisia glue,the mol ratio of NaOH and Artemisia glue (etherification reaction phase) were also studied.The most optimal process condition of the preparation of carboxylmethyl Artemisia glue was determined by orthogonal test:the alkalifying time 1.5h,the etherification temperature 35℃,the concentration of Artemisia glue 40g/L ,the mol ratio of NaOH and Artemisia glue 1∶1, the etherification time 3h,the etherification temperature 60℃, the volume fraction of alcohol 75%, the mol ratio of chloroacetic acid and Artemisia glue 0.6∶1,the mol ratio of NaOH and Artemisia glue 0.7∶1.Under these conditions,the DS of carboxylmethyl Artemisia glue was 0.4982,reaction efficiencyion was 83.03%.
Due to the introduction of carboxylmethyl group, the content of water-insoluble components decreased from 56.02% to 15.01% and the rate of water absorption increased from 13.02% to160.08% as the DS of carboxylmethyl Artemisia glue was 0.4982.Carbxylmethyl Artemisia glue was a kind of thixotropy.Apparent viscosity increased with the increase of concentration.And its apparent viscosity decreased with the increase of temperature.When the pH increased,the apparent viscosity increased firsly and then decreased.The NaCl made the apparent viscosity of carbxylmethyl Artemisia glue decreased and the sucrose affected the apparent viscosity smoothly.Besides,there were three strong peaks appeared in 1730cm~(-1), 1382cm~(-1)and 1254cm~(-1) in the Infra-red spectrometris of arbxylmethyl Artemisia glue,it indicated that the arbxylmethyl Artemisia contain -C=O,-CH2 and -C-O.So the differences of the Infra-red spectrometris of Artemisia glue and carbxylmethyl Artemisia glue showed that the carboxylmethyl group had been inserted into Artemisia glue.
The carboxylmethyl group introduced gave Artemisia glue some new character, so it could be used in quick-frozen dumpling.When the carbxylmethyl Artemisia glue was used inside of dumpling,the optimum condition was as follow: the DS of carboxylmethyl Artemisia glue 0.4982,the content of carboxylmethyl Artemisia glue 0.2%.In this condition the frost shattering rate decreased 17.14%.When the carbxylmethyl Artemisia glue was used in the skin of dumpling,the optimum condition was as follows: the DS of carboxylmethyl Artemisia glue 0.4982,the content of carboxylmethyl Artemisia glue 0.2%~0.25%. In this condition the frost shattering rate decreased 42.85%.
通过单因素实验分别研究了碱化反应阶段的碱化时间、碱化温度、沙蒿胶的质量浓度、NaOH与沙蒿胶的摩尔比和醚化反应阶段的醚化时间、醚化温度、乙醇的体积分数、氯乙酸与沙蒿胶的摩尔比、NaOH与沙蒿胶的摩尔比对取代度和反应效率的影响,在此基础上,通过正交实验确定了制备羧甲基沙蒿胶的最佳工艺条件。实验结果表明,碱化反应阶段的最佳工艺条件为:碱化时间为1.5h,碱化温度为35℃,沙蒿胶的质量浓度为40g/L(以沙蒿胶的干基计算),NaOH与沙蒿胶的摩尔比为1∶1;醚化反应阶段的最佳工艺条件为:醚化时间为3h,醚化温度为60℃,乙醇的体积分数为75%,氯乙酸与沙蒿胶的摩尔比为0.6∶1,NaOH与沙蒿胶的摩尔比为0.7∶1。在最优的工艺条件下,得到的羧甲基沙蒿胶的取代度为0.4982,反应效率为83.03%。
对羧甲基沙蒿胶的性质进行了分析,结果表明:通过羧甲基化,当羧甲基沙蒿胶的取代度为0.4982时,其水不溶物含量由原来的56.02%降为15.01%,吸水率由原来的13.02%上升到160.68%;羧甲基沙蒿胶溶液的粘度随着剪切速率的增加而降低,属于非牛顿流体,其表观粘度随着羧甲基沙蒿胶质量分数的增加而增加,温度对羧甲基沙蒿胶粘度的影响随着取代度的增加而呈明显的下降趋势,羧甲基沙蒿胶溶液的粘度随着pH的增加先升高后降低,NaCl会降低羧甲基沙蒿胶溶液的粘度而蔗糖使其粘度升高。另外,通过红外光谱实验得出,改性后的沙蒿胶分别在1730cm~(-1)、1382cm~(-1)和1254cm~(-1)处出现了很强的吸收峰,表明改性后体系中含有-C=O、-CH2和-C-O,因此从原沙蒿胶与改性后的羧甲基沙蒿胶在红外光谱图上的区别可以得出羧甲基已经成功地接到了沙蒿胶上。
将羧甲基沙蒿胶应用于速冻水饺,通过实验确定了较佳的工艺条件,将羧甲基沙蒿胶应用于饺子馅的工艺条件为:取代度为0.4982,添加量为馅料质量的0.2%,冻裂率下降17.14%;将羧甲基沙蒿胶应用于饺子皮的工艺条件为:取代度为0.4982,添加量为面粉质量的0.2%～0.25%,冻裂率下降42.85%。
It was studied in this thesis the preparation of Artemisia glue, under the condition of alkali, chloroacetic acid was used as etherification agent and the properties, structures and application in quick-frozen dumpling were researched too.
In the single factor experiments, the affects of degree of substitution(DS) and reaction efficiency(RE) by some factors,which included,the alkalifying time,the alkalifying temperature,the concentration of Artemisia glue,the mol ratio of NaOH and Artemisia glue (alkalified reaction phase),the etherification time,the etherification temperature,the volume fraction of alcohol,the mol ratio of chloroacetic acid and Artemisia glue,the mol ratio of NaOH and Artemisia glue (etherification reaction phase) were also studied.The most optimal process condition of the preparation of carboxylmethyl Artemisia glue was determined by orthogonal test:the alkalifying time 1.5h,the etherification temperature 35℃,the concentration of Artemisia glue 40g/L ,the mol ratio of NaOH and Artemisia glue 1∶1, the etherification time 3h,the etherification temperature 60℃, the volume fraction of alcohol 75%, the mol ratio of chloroacetic acid and Artemisia glue 0.6∶1,the mol ratio of NaOH and Artemisia glue 0.7∶1.Under these conditions,the DS of carboxylmethyl Artemisia glue was 0.4982,reaction efficiencyion was 83.03%.
Due to the introduction of carboxylmethyl group, the content of water-insoluble components decreased from 56.02% to 15.01% and the rate of water absorption increased from 13.02% to160.08% as the DS of carboxylmethyl Artemisia glue was 0.4982.Carbxylmethyl Artemisia glue was a kind of thixotropy.Apparent viscosity increased with the increase of concentration.And its apparent viscosity decreased with the increase of temperature.When the pH increased,the apparent viscosity increased firsly and then decreased.The NaCl made the apparent viscosity of carbxylmethyl Artemisia glue decreased and the sucrose affected the apparent viscosity smoothly.Besides,there were three strong peaks appeared in 1730cm~(-1), 1382cm~(-1)and 1254cm~(-1) in the Infra-red spectrometris of arbxylmethyl Artemisia glue,it indicated that the arbxylmethyl Artemisia contain -C=O,-CH2 and -C-O.So the differences of the Infra-red spectrometris of Artemisia glue and carbxylmethyl Artemisia glue showed that the carboxylmethyl group had been inserted into Artemisia glue.
The carboxylmethyl group introduced gave Artemisia glue some new character, so it could be used in quick-frozen dumpling.When the carbxylmethyl Artemisia glue was used inside of dumpling,the optimum condition was as follow: the DS of carboxylmethyl Artemisia glue 0.4982,the content of carboxylmethyl Artemisia glue 0.2%.In this condition the frost shattering rate decreased 17.14%.When the carbxylmethyl Artemisia glue was used in the skin of dumpling,the optimum condition was as follows: the DS of carboxylmethyl Artemisia glue 0.4982,the content of carboxylmethyl Artemisia glue 0.2%~0.25%. In this condition the frost shattering rate decreased 42.85%.
引文
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