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Study On The Identification And Content Determination Methods Of Anthocyanins In Blueberry

Posted on:2021-10-11Degree:MasterType:Thesis
Country:ChinaCandidate:R J HuFull Text:PDF
GTID:2481306518990329Subject:Applied Chemistry
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This thesis aimed at the synthesis and application of ten new N,N-diethylacetate series azo disperse dyes.First,we used 3-amino-4-methoxyacetanilide and 3-acetamidoaniline as raw materials and ethyl chloroacetate as the alkylating reagent,explored the types of catalysts,acid binding agents,reaction time and feeding methods.The effect of the reaction,and the structural characterization of the two N,N-diethylacetate-based aromatic amine dye intermediates synthesized.Next,we used two N,N-diethylacetate-based aromatic amines as coupling components,2-amino-3,5-dinitrothiophene,3-amino-5-nitro-2,1-benzene Five novel aromatic amines such as isothiazole,4-nitroaniline,2,4-dinitro-6-chloroaniline were used as the diazo component,and ten new N,N-bis were synthesized through the diazotization-coupling reaction.The ethyl acetate-based series of azo disperse dyes were examined by ultraviolet-visible absorption spectrum for the maximum visible absorption wavelength and molar absorption coefficient of these ten disperse dyes,and their ratio shift values were determined.And other means to characterize their molecular structure.And we took the disperse dye(represented by A1B3)synthesized by 3-(N,N-diethylacetate)amino-4-methoxyacetanilide and 4-nitroaniline as an example,the factors affecting the synthesis reaction were discussed,optimized the synthesis process.Finally,the dyeing shade,dyeing percentage and dyeing fastness of these ten azo disperse dyes on polyester fabric and benzyl wood powder were explored.The conclusions were as follows:1?We used 3-amino-4-methoxyacetanilide and 3-acetamidoaniline as raw materials and ethyl chloroacetate as an alkylating reagent,two N,N-diethylacetate aromatic amine dye intermediates were synthesized The suitable acid binding agent was sodium carbonate,the best catalyst was sodium bromide,and the effective antioxidant was zinc powder.2?We used 3-amino-4-methoxyacetanilide and 3-acetamidoaniline as raw materials and ethyl chloroacetate as an alkylating reagent to synthesis two N,N-diethylacetate-based dye intermediates,and the optimized process was:aromatic amine:chloroacetate:sodium carbonate is 1:5:1.1(mol),after refluxing for 2 h,add 10%catalyst sodium bromide and0.5%antioxidant zinc powder(m%),then proceed Water was refluxed for 2 h to obtain two dye intermediates with a content(HPLC)of more than 99.4%and a yield of more than97.7%.The analysis of ultraviolet spectrum,infrared spectrum,nuclear magnetic resonance hydrogen spectrum and mass spectrometry showed that these two N,N-diethylacetate-based aromatic amine dye intermediates were the target products.3?We used 3-(N,N-diethylacetate)amino-4-methoxyacetanilide and 3-(N,N-diethy lacetateacetanilide as coupling components,2-amino-3,5-dinitrothiophene,3-amino-5-nitro-2,1-benzisothiazole,2,4-nitroaniline,2,4-dinitro-6-chloroaniline and 2,4-Dinitro-6-brom oaniline as a diazo component.Ten diethyl acetate-based disperse dyes were synthesized through diazotization-coupling reaction,and the yield was 87.6%-94.8%;Nuclear magnetic resonance hydrogen spectroscopy and mass spectrometry analysis confirmed the target product.4?The largest of ten disperse dyes synthesized with 3-(N,N-diethylacetate)amino-4-methoxyacetanilide and 3-(N,N-diacetateacetanilide)as coupling components.The visible absorption wavelength was from 493 nm to 655 nm(acetone).A1 series disperse dyes with-OCH3 substituents on the coupling component benzene ring were 20 nm longer than the maximum visible absorption wavelength of the A2 series dyes without-OCH3 substituents Disperse dyes containing thiophene rings were longer than the maximum absorption wavelength of azo disperse dyes containing benzene rings;the molar absorption coefficient at the maximum visible absorption wavelength was between 1.17×104?2.86×104,reflecting the characteristics of high color intensity.5?2-amino-3,5-dinitrothiophene and 3-(N,N-diethylacetate)amino-4-methox yaceta nilide were used as the diazo component and the coupling component.The process was:diazotization reaction adopts phosphoric acid:sulfuric acid(v:v)is 2:1 as medium,2-amino-3,5-dinitrothiophene and Na NO2 molar ratio was 1:1.05,diazotization temperature0?5?;when the diazo component:the molar ratio of the coupling component was 1:1.0?1.1,the coupling temperature is-5??5?,the coupling time was 8-9 hours,the purity can be obtained 99.0%,the yield was 87.6%dye.6?Under high temperature and high pressure,the dye concentration was 1.0%(owf),the bath ratio was 100:2,the color of ten N,N-xylyl disperse dyed polyester fabrics was divided into blue green,bright green,bright red,blue Violet,blue-violet,brilliant blue,brilliant blue,red-orange,brilliant purple and brilliant purple,and bright colors;the dyeing percentage of polyester fabrics dyed on polyester fabric was 86.8%?95.6%,the dyeing rate of five A1series dyes All are lower than the corresponding dyeing percentage of each of the six A2series dyes;the washed(sticky)color fastness of dyed polyester fabric was 4?5,and the sun fastness was 6?7,reflecting the high wash fastness and High light fastness characteristics.7?The B1 and B2series dyed polyester fabrics with heterocyclic structure had a soaping color fastness of 5 and the sun fastness was 7 grades.They were better than the other six disperse dyed polyester fabrics without a heterocyclic structure.The soaping color fastness and sunlight fastness were 0.5 to 1 grade higher.Heterocyclic-bis-ethyl acetate disperse dyes not only had bright colors,but also more excellent color fastness,and had good application prospects.8?Under high temperature and high pressure,the dye concentration was 1.0%(owf),the bath ratio was 100:2,and the color of ten N,N-diethylacetate-based disperse dyes for benzyl wood powder was divided into blue green,green,and jujube.Red,blue-violet,blue-violet,blue-violet,blue-violet,orange,purple,and purple,but slightly darker than the same dye dyed polyester fabric;the dyeing percentage of benzyl wood powder dyed on the dye was92.9%-98.6%,They are higher than the dyeing percentage of dyed polyester fabric with the same dye 86.8%?95.6%;the washed(sticky)color fastness of dyed benzyl wood powder was 4 to 5 grades,and the washed(sticky)color fastness of dyed polyester fabric The degree was basically the same.
Keywords/Search Tags:ethyl chloroacetate, ethyl acetate group, Azo disperse dyes, dyeing, benzyl wood powder
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