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A kind of preparation technology of alkyl glycoside

An alkyl glucoside and a preparation process technology, which is applied in the field of preparation of dodecyl glucoside, can solve the problems of easy agglomeration of glucose, shortened reaction time and the like, and achieves shortened reaction time, simplified process, environmental protection and resource efficiency. The effect of using

Inactive Publication Date: 2018-11-16
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention provides a preparation process of alkyl glucosides. For the first time, the water vapor in the reaction system is taken out in time by air ventilation method, which breaks the reaction balance, improves the reaction efficiency, and solves the problem that glucose is easy to agglomerate during the reaction process; The compound acid is used as a catalyst to improve the catalytic efficiency, greatly shorten the reaction time, simplify the process, lower the production cost, and significantly improve the product performance

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Add 93g of n-dodecanol and compound acid into a 500mL three-necked round bottom flask, install an electric stirrer, add 18g glucose under stirring, turn on the vacuum pump, and pump water at 80℃ for 1h;

[0035] The mass ratio of glucose to the compound acid is 1:0.018; the molar ratio of p-toluenesulfonic acid, phosphoric acid and sulfuric acid in the compound acid is 1:0.18:0.24; the mass concentration of the sulfuric acid solution is 50%.

[0036] (2) The temperature is raised to 110°C, and the glycosylation reaction is performed at a pressure of 50.00KPa for 40 minutes;

[0037] (3) Adjust the pH value of the reactant to 9-10, raise the temperature to 130°C, and extract the free alcohol at a pressure of 30.15KPa;

[0038] (4) Add hydrogen peroxide with a mass concentration of 20% for bleaching;

[0039] (5) Drying to obtain a creamy white cream solid of alkyl glycoside.

[0040] The color of the product is milky white (first-class product), the foam height of the one-thous...

Embodiment 2

[0042] (1) Add 74g of n-dodecanol and compound acid to a 500mL three-necked round bottom flask, install an electric stirrer, add 18g glucose under stirring, turn on the vacuum pump, and pump water at 90°C for 0.5h;

[0043] The mass ratio of glucose and compound acid is 1:0.030; the molar ratio of p-toluenesulfonic acid, phosphoric acid and sulfuric acid in the compound acid to the compound acid is 1:0.24:0.24; the mass concentration of the sulfuric acid solution is 50%.

[0044] (2) The temperature is raised to 105°C and the glycosylation reaction is performed at 45.11KPa for 60 minutes;

[0045] (3) Adjust the pH value of the reactant to 10-11, heat up to 135°C, and extract free alcohol at a pressure of 24.15KPa;

[0046] (4) Add hydrogen peroxide with a mass concentration of 40% for bleaching;

[0047] (5) Drying to obtain a creamy white cream solid of alkyl glycoside.

[0048] The color of the product is milky white (first-class product), the foam height of the one-thousandth aqueous...

Embodiment 3

[0050] (1) Put 55.8g of n-dodecanol and compound acid into a 500mL three-necked round bottom flask, install an electric stirrer, add 18g glucose under stirring, turn on the vacuum pump, and pump water at 85℃ for 1h;

[0051] The mass ratio of glucose and compound acid is 1:0.020; the molar ratio of p-toluenesulfonic acid, phosphoric acid and sulfuric acid in the compound acid in the compound acid is 1:0.24:0.18; the mass concentration of the sulfuric acid solution is 40%.

[0052] (2) The temperature is raised to 100°C, and the glycosylation reaction is performed at a pressure of 53.41KPa for 80 minutes;

[0053] (3) Adjust the pH value of the reactant to 7-9, raise the temperature to 130°C, and extract the free alcohol at a pressure of 37.45KPa;

[0054] (4) Add hydrogen peroxide with a mass concentration of 30% for bleaching;

[0055] (5) Drying to obtain a creamy white cream solid of alkyl glycoside.

[0056] The color of the product is milky white (first-class product), the foam heig...

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Abstract

The invention discloses a preparing process for alkyl glycoside, and belongs to the technical field of fine chemical engineering. The preparing process includes the following steps that 1, n-dodecanol and composite acid are added into a reaction device, glucose is added under the stirring condition, and a vacuum pump is started and used for pumping water for 0.5-2 h at the temperature of 80 DEG C-90 DEG C; 2, the temperature rises to 100 DEG C-120 DEG C, and a glycosylation reaction is carried out for 40-80 min at the pressure of 40.11-53.41 KPa; 3, the pH value of reactants is adjusted to be 7-11, and free alcohol is removed by suction after the temperature rises to 130 DEG C-135 DEG C; 4, bleaching is carried out; 5, drying is carried out. For the first time, an air introducing method is adopted to take away steam in the reaction system in time, reaction balance is broken, the reaction efficiency is improved, and the problem that glucose is prone to caking in the reaction process is solved. As the composite acid is adopted as a catalyst, the catalysis efficiency is improved, the reaction time is greatly shortened, the process is simplified, the production cost is low, and the performance of alkyl glycoside is obviously improved.

Description

Technical field [0001] The present invention relates to the technical field of fine chemicals, in particular to a preparation method of lauryl glucoside, which can be widely used in the fields of daily chemicals, food, medicine and the like. Background technique [0002] In recent years, due to the increasingly severe environmental problems, environmental protection issues have gradually become the focus of people's attention. my country has also put forward higher requirements for environmental protection. Some non-degradable and phosphorus-rich surfactants have caused great harm to the environment. Surfactants are mainly composed of non-polar hydrophobic groups and polar hydrophilic groups. There are many types of surfactants. According to different hydrophilic groups, surfactants are mainly divided into four categories: cationic, anionic, amphoteric, and nonionic. Among them, anionic surfactants are currently the largest and most widely used type of surfactants. The weakness...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/04C07H1/00C07H1/06
Inventor 牛春梅吴顺伟李绍英
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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