A method for preparing sucralose-6-ethyl ester
A technology of sucralose and ethyl ester, which is applied in the preparation of sugar derivatives, chemical instruments and methods, sugar derivatives, etc., can solve the problems of affecting product quality, low selectivity, and high energy consumption in production, and achieve the suppression of polychlorination The generation of by-products, the simple process route, and the effect of improving the dispersion
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Embodiment 1
[0044] 57.5g Pd(dba) 2 , 26.6g of BINAP, 31.9g of 2,2-bipyridine were mixed in 500g of distilled water, heated to 60°C and stirred for 6h to fully mix, and 37.2g of 4A molecular sieves were added under stirring to obtain suspension A; Make 25wt% sodium hydroxide solution in water to be the alkaline precipitant B, respectively heat the suspension A and the alkaline precipitant B to 30°C, and slowly add the alkaline precipitant B to the suspension In A, the pH of the system is 9, and the reaction temperature of the precipitation process is controlled at 30°C; then the slurry is obtained after aging at 75°C for 4h; the slurry is filtered, washed with deionized water, and the filter cake is dried at 115°C for 18h, and Calcined at 350°C for 20 hours, crushed, and pressed into tablets to obtain catalyst 1.
[0045]After ICP analysis, it is determined that in Catalyst 1, by mass (if there is no special label, the crystal water of the above-mentioned metal salt raw material is not co...
Embodiment 2
[0047] Mix 102.2g of bis(tri-tert-butylphosphine)palladium, 49.7g of dppp, and 56.8g of quinoline in 1000g of distilled water, raise the temperature to 80°C and stir for 4 hours to fully mix, then add 49.7g of kaolin while stirring to obtain a suspension A; Dissolve sodium carbonate in water to form a 25wt% sodium carbonate solution, which is the alkaline precipitant B. Heat the suspension A and the alkaline precipitant B to 40°C respectively, and drop the alkaline precipitant B slowly Add it to suspension A until the pH of the system is 10, control the reaction temperature of the precipitation process at 40°C; then age at 85°C for 3 hours to obtain a slurry; filter the slurry, wash with deionized water, and filter the cake at 130°C ℃ drying for 9 hours, and calcination at 500 ℃ for 7 hours, crushing and tableting to obtain catalyst 2.
[0048] After ICP analysis, it was determined that in the catalyst 2, the following components accounted for the percentages of the total mass...
Embodiment 3
[0050] Mix 153.3g of bis(tri-tert-butylphosphine)palladium, 85.9g of BINAP, and 66.3g of diphenyl disulfide in 1000g of distilled water, raise the temperature to 50°C and stir for 7 hours to fully mix, then add 61.4g of silicon dioxide under stirring Mix to obtain suspension A; dissolve ammonium carbonate in water to form a 25wt% ammonium carbonate solution, which is alkaline precipitant B, heat suspension A and alkaline precipitant B to 35°C respectively, and Precipitant B was slowly added dropwise to suspension A until the pH of the system was 11, and the reaction temperature of the precipitation process was controlled at 35°C; then the slurry was obtained after aging at 65°C for 5 hours; the slurry was filtered, washed with deionized water, and The filter cake was dried at 120° C. for 12 hours, calcined at 400° C. for 10 hours, crushed and pressed into tablets to obtain Catalyst 3 .
[0051] After ICP analysis, it was determined that in the catalyst 3, the following compone...
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