The Preparation Technology And Process Analysis Of Sucralose By Chlorination And Deacylation

Sucralose is a kind of sucral chloride derivatives,which is currently considered one of the most powerful sweetener.As a high sweetness,low calorific value,and stable physicochemical property,sucralose has been widely used at home and abroad.3Due to the increased demand for high purity of sucralose in the market,which bring forward higher request to the synthetic process and analyze method.As the rapid development of chemometrics and analytical instruments,it provides a powerful research tool for the complex multi-component chemical system to fast,convenient,and efficient analysis.In this paper,sucralose was producted with sucrose-6-acetate through the single group protection method,and then further study the synthesis and crystallization conditions,proposing a approximate linearity quantitative method,which based on the change of spectral intensity of light channel and background.According to the the traditional KBr compaction method,sucralose and synthetic products were quantitative analysed on account of mid infrared spectra combined with spatial vector.The main contents are as follows:(1)Chlorination process technology:Sucrose-6-acetate DMF solution as raw material,chlorinated reagent Vilsimeier reagent preparation of sucralose-6-acetate,and then slowly adding sucrose-6-acetic acid Ester,system research and optimization of chlorination stage of the material ratio,trichloride temperature,time and other factors.The results showed that n(SOCl2):n(sucrose-6-acetate)=10:1,V(DMF):m(sucrose-6-acetate)=13:1,110?,the reaction time is 4 h,the obtained sucralose-6-acetate is the best result.The extract amount of ethyl acetate is 4 times,the amount of extraction solution is 1/2,the extraction efficiency can reach 97.26%,through the ethyl acetate in the crystallization of more than 95%purity.(2)Deacylation process:The chlorinated sucralose-6-acetate was alcohol-eluted in a sodium methoxide-methanol system,neutralized with an H~+cation exchange resin,and used in its aqueous solution The results showed that the deacidification temperature was 35?,the reaction time was 3 h,and the reaction time was 3 h,and the reaction temperature was 35?and the reaction time was 3 h,PH9.0,at this time the best deacylation effect;by melting point determination,infrared spectral spectrum to confirm the structure,through the high performance liquid chromatography to determine the purity and calculate the yield,for the product of sucralose crystallization process were explored,The results showed that ethyl acetate was used as the extraction agent,the extraction efficiency was the best and the purity was above99.23%.The sucralose crystallization process was purified.The aqueous solution of sucralose was extracted with ethyl acetate and butyl acetate respectively.The aqueous phase was collected and the aqueous phase was collected in water and cooled at 4°C to recrystallize and dried in vacuo to determine purity by HPLC.The purity of sucrose was 99.95%or more.(3)Quantitative analysis based on mid-infrared spectroscopy:By discussing the change of spectral intensity of light channel and background,a new approximation linearity is proposed by combining the space vector angle method.According to the traditional KBr pressure Direct synthesis of product of sucralose by.The correlation coefficient between the predicted value and the measured value is more than 99.5%and the relative error is less than 8.0%,which indicates that this method can overcome the influence of factors such as multiplication and addition in the spectrum measurement process to achieve the rapid detection of process quality.