Neotame And Its Derivatives, Industrial Design And The Comprehensive Utilization Of Nitro-anthraquinone Residue

The content of this thesis consist two parts.1.The synthesis of N-alkyl derivatives aspartameIn recent years,it has received more and more people's attention to the enhancement of life quality.Especially excessively ingesting the sugar could cause adiposity which would lead to various diseases.A sweeter with high sweetness and low heat should urgently be developed.Dipeptide sweeters with good sweetness feeling and low heat were the substitute of sucrose,which have received more and more favour by consumers.In this paper,N-[N-(3,3-dimethylbutyl)-L-aspartyl]-L-phenylalanine 1-methyl ester and N-[N-(3,3-dimethylamyl)-L-aspartyl]-L-phenylalanine 1-methyl ester were simply synthesized by the hydrogenation of aspartame and alkyl aldehyde.Generally, the synthetic method was showed as follows:3,3-dimethylbutyl(amyl)chloride was produced by tert-butyl(amyl)chloride and ethylene with the catalyst of aluminium chloride at ice-bath.3,3-dimethylbutyl(amyl)aldehyde was preparaed by the oxidation reaction of 3,3-dimethylbutyl(amyl)chloride.N-alkyl aspartame derivatives were produced by the hydrogenation reaction of aspartame and 3,3-dimethylbutyl (amyl)aldehyde with the catalyst of Pd/C to give high yields.Main innovations of the paper:1)Two N-alkyl aspartame derivatives were synthesized by a few steps with the original material——tert-butyl(amyl)alcohol.2)Combined with the practical production,a reasonable pilot programme of N-alkyl aspartame derivatives was designed and successfully applied into industrialized production.2.Comprehensive utilization of nitroanthraquinone waste residueAnthraquinone dyestuff is the second largest series beside the azo dyes.It has the good property of bright colour,high fastness,no fading and so on.Nitroanthraquinone is an important material in the dyestuff industry.During the dyestuff production,there are a lot of nitroanthraquinone derivatives in the waste residue.During the dyestuff production,there are a lot of nitroanthraquinone derivatives in the waste residue,including 1-Nitroanthraquinone,2-Nitroanthraquinone,1,5-,1,8-, 1,6- and 1,7-Dinitroanthraquinone and Anthraquinone.If they are discarded in the environment,or burnt,they will cause serious pollution.Procession of Purification of 1-nitroanthraquinone:The waste residue contains 35-42%1-nitroanthraquinone.This work puts emphasis upon the purification and separation of the waste residue.In the study,the treatment including two methods such as extracting and separating with organic solvent as well as sodium nitrates solution.After treated by the organic solvent,we gained a preferable effect.After we studied of one or two kinds of organic solvent,dichloride ethanes and chlorobenzene,various proportion of solvent,various proportion of initiators and the time of cooling,we found a perfect way of purification 1-nitroanthraquinone and put into industrialization successfully.This article contains preparation 80%1-aminoanthraquinone and 1-methylamino-anthraquinone from 80%1-nitroanthraquinone purified by waste residue.The reduction by Na₂S solution could give a better result than the directly substitution by NH₃.We prepared 1-methylaminoanthraquinone,which is an important disperse dye and solvent dye,by the reaction between 1-nitroanthraquinone and methylamine catalyzed by inorganic base.After recrystallization,we could get bright red dye, containing 80%1-methylaminoanthraquinone by HPLC.Process of nitration of the waste residue:Lots of important dark anthraquinone dyestuff such as blue,green and brown et al are prepared by 1,5- and/or 1,8-dinitroanthraquinone which are very important in the dye industry.This article puts emphasis upon the nitration of the waste residue.The nitration includes four methods:nitration in sulfate,nitration by pure nitrate,nitration by mixed acid and nitration in organic solvent.We prepared a purple disperse dye, which could dye Polypropylene and Cellulose acetate,by dinitroanthraquinone.It has perfect Wash fastness and Sublimation fastness,but bad light fastness.