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Method for preparing alkyl polyglucoside (APG) through microwave-ultrasonic wave concerted catalysis
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A technology of alkyl glycosides and synergistic catalysis, which is applied in chemical instruments and methods, preparation of sugar derivatives, sugar derivatives, etc., to achieve fast reaction speed, short reaction time, and high glucose conversion rate
Active Publication Date: 2013-12-18
ZANYU TECH GRP CO LTD
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Embodiment 1
[0020] Add 54gC to a 100mL three-necked flask 12 / 14 Fatty alcohol, 10g glucose, placed in the center of the microwave reactor, installed an electric stirring rod, set the temperature to 115℃ for 5min, vacuum dehydration for 15min, then add 0.1g alkylbenzene sulfonic acid, set the microwave radiation power of 150W , Under the condition of 6.0KPa absolute pressure, react for 30min. After the reaction, when the temperature is lowered to 80°C, neutralize with sodium bicarbonate to pH=8, raise the temperature to 140°C, and the absolute pressure is 6.5KPa, and carry out reduced pressure distillation and dealcoholization to obtain crude APG product with a conversion rate of 69% .
Embodiment 2
[0022] In a 100mL three-necked flask, add 54gC 16 / 18 Fatty alcohol, 12g glucose, placed in the center of microwave reactor, installed electric stirring rod, heated to 118℃ in 5min, vacuum dehydrated, then added 0.1g sodium bisulfate, set microwave radiation power of 400W, absolute pressure of 6.5KPa Under the conditions, the reaction time is 60min. After the reaction, after the temperature is lowered to 70°C, the pH is neutralized with sodium carbonate to pH=8.5, the temperature is increased to 130°C, and the absolute pressure is 6.5KPa, and the alcohol is dealcoholized under reduced pressure to obtain the crude APG product with a conversion rate of 95%.
Embodiment 3
[0024] In a 100mL three-necked flask, add 60gC 8 / 10 Fatty alcohol, 10g glucose, placed in the center of the microwave reactor, installed the ultrasonic device, heated to 120℃ in 5min, vacuum dehydrated, then added 0.5g p-toluenesulfonic acid, set ultrasonic power 600W, magnetic stirring, 500W microwave radiation Under the condition of power and absolute pressure of 6.0KPa, react for 30min. After the reaction, after the temperature is lowered to 60°C, neutralize to pH=9 with sodium hydroxide, raise the temperature to 135°C, the absolute pressure is 4.5KPa, and carry out reduced pressure distillation and dealcoholization to obtain crude APG product with a conversion rate of 99% .
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Abstract
The invention relates to a method for preparing alkyl polyglucoside (APG) through microwave-ultrasonic wave concerted catalysis, and aims to provide a method having the advantages of high reaction speed, high conversion rate, small environmental influence and the like. The technical scheme comprises the following steps: a, adding glucose and fatty alcohol into a container according to a mol ratio of 1:(2-10), stirring, carrying out microwave heating for 5 minutes under ultrasonic wave radiation conditions to 110-120 DEG C, and carrying out vacuum dewatering for 15 minutes at the absolute pressure of 1.5-6.5 KPa; b, adding an acidic catalyst, and reacting for 30-90 minutes at the absolute pressure of 1.5-6.5 KPa; c, when the temperature is cooled to 50-80 DEG C after the reaction, neutralizing the acidic catalyst with a neutralizer until the pH value is 8-11; and d, raising the temperature to 120-200 DEG C, and carrying out reduced pressure distillation for dealcoholization at the absolute pressure of 1.5-6.5 KPa, thus obtaining a crude APG product.
Description
Technical field [0001] The invention belongs to the field of surface active agent preparation, and particularly relates to a method for preparing alkyl glycosides through microwave-ultrasound cooperative catalysis. Background technique [0002] Alkyl polyglycoside (APG) is a new type of surfactant developed in the late 1980s and early 1990s. It has many advantages of both nonionic and anionic surfactants. It not only has low surface tension but high activity. , Strong detergency, rich, delicate and stable foam, good compatibility with other surfactants, low skin and eye irritation, good biodegradation, non-toxic, good compatibility, and no pollution to the environment. It is widely used in detergents, industrial emulsifiers, cosmetics, food and pharmaceutical industries. Because of its synthetic raw materials and performance characteristics, it is known as a new generation of mild "green" surfactants, and it is the only variety that can truly be called "world-class" surfactants ...
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