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Preparation method of glucoside cationic surfactant

A surfactant and cation technology, which is applied in the field of preparation of alkyl glycoside derivatives, can solve the problems of lack of detailed analysis of reaction degree, low final yield, long reaction time, etc., achieving good separation effect and shortening reaction time. time, the effect of improving conversion rate

Inactive Publication Date: 2010-12-29
SHANGHAI FINE CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Combining the previous methods, the reaction time is very long, and the degree of reaction of each step has not been analyzed in detail, resulting in a low final yield

Method used

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  • Preparation method of glucoside cationic surfactant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Into a 250 mL four-necked flask equipped with a condenser, a thermometer and a stirrer, 36.0 g of anhydrous glucose, 44.2 g of 3-chloro-1,2-propanediol and 0.3 g of p-toluenesulfonic acid were added. React at a pressure of 200 mmHg and a temperature of 90° C. for 60 minutes to obtain 76.6 g of a light yellow transparent viscous liquid, wherein the conversion rate of glucose is 99.6%. Neutralize to PH≈7 with saturated NaOH aqueous solution. Then the neutralized solution was added to a molecular still, the temperature was controlled to be 100° C., and the pressure was 1 mba to remove excess 3-chloro-1,2-propanediol. 3-Chloro-2-hydroxypropyl glucoside was obtained as a solid. Dissolve the chloroglycoside in water to prepare a 50% aqueous solution.

[0028] In a 250mL four-neck flask equipped with a condenser, a thermometer and a stirrer, add 65g of the above chloroglucoside solution, stir and heat. When the reaction temperature was 50° C., a mixed solution of 15.5 g of ...

Embodiment 2

[0030] Into a 250 mL four-necked flask equipped with a condenser, a thermometer, and a stirrer, 36.0 g of anhydrous glucose, 66.3 g of 3-chloro-1,2-propanediol, and 0.3 g of sulfosuccinic acid were added. React at a pressure of 200 mmHg and a temperature of 110° C. for 50 minutes to obtain 96.2 g of a light yellow transparent viscous liquid, wherein the conversion rate of glucose is 99.5%. Neutralize with saturated KOH aqueous solution to pH ≈ 8, then add the neutralized solution into a molecular still, control the temperature at 160°C, and pressure 3mba to remove excess 3-chloro-1,2-propanediol to obtain 3 - Chlorinated 2-hydroxypropyl glucoside. Dissolve the chloroglycoside in water to prepare a 40% aqueous solution.

[0031] In a 250mL four-neck flask equipped with a condenser, a thermometer and a stirrer, add 81g of the above chloroglycoside aqueous solution, stir and heat. When the reaction temperature was 50° C., a mixed solution of 11 g of dodecyldimethyl tertiary ami...

Embodiment 3

[0033] Into a 250 mL four-necked flask equipped with a condenser, a thermometer, and a stirrer, 36.0 g of anhydrous glucose, 56.7 g of 3-chloropropanol, and 0.20 g of p-toluenesulfonic acid were added. React at a pressure of 200 mmHg and a temperature of 90° C. for 120 minutes to obtain 86.4 g of light yellow transparent viscous liquid, wherein the conversion rate of glucose is 99.7%. Neutralize to pH ≈ 7 with saturated NaOH aqueous solution, then add the neutralized solution into a molecular still, control the temperature at 150 ° C, and the pressure at 2.8 mba to remove excess 3-chloropropanol to obtain solid 3-chloropropanol Propyl glucoside. Dissolve the solid 3-chloropropyl glucoside in water to prepare a 50% aqueous solution.

[0034] In a 250mL four-neck flask equipped with a condenser, a thermometer and a stirrer, add 65g of the above-mentioned 3-chloropropyl glucoside aqueous solution, stir and heat. When the reaction temperature was 50° C., a mixed solution of 8.8 ...

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Abstract

The invention discloses a preparation method of a glucoside cationic surfactant, which is characterized by comprising the following steps: (1), adding raw materials including glucose, chlorohydrins and a catalyst in to a reactor in a ratio of 1:2-5:0.002-0.01 and performing a dehydration reaction under a reduced pressure for 30 to 120 minutes at 80 to 110 DEG C to obtain yellowish or colorless transparent sticky liquid; (2) neutralizing the reaction product with a neutralizer till the pH value of the reaction product is 7 to 8 and performing molecular distillation at 100 to 180 DEG C and under 1 to 3MPa to obtain solid chlorinated glucoside; and (3) preparing 30 to 60 percent aqueous solution of the chlorinated glucoside, slowly adding tertiary amine, which is added with an organic solvent, into the solution of the chlorinated glucoside in a molar ratio of 1:0.5-1.0 and performing a reaction at 60 to 90 DEG C and under normal pressure for 2 to 10 hours to obtain transparent solution of the glucoside cationic surfactant.

Description

technical field [0001] The invention relates to a preparation method of an alkyl glycoside derivative, in particular to a preparation method of a glycoside cationic surfactant. Background technique [0002] Glycoside quaternary ammonium salt is a kind of green surfactant produced by natural renewable glucose. It is not only rich in raw materials, cheap, but also has excellent performance and good biodegradability. In recent years, it has gradually attracted the attention of scholars at home and abroad. Such as U.S. Patent (US 5773595) utilizes dodecyl glucoside and quaternization reagent 3-chloro-2-hydroxypropyltrimethylammonium chloride to react under the catalysis of NaOH, and one-step method has prepared glucose-based cationic surfactant . Although the method is simple in technique, the reaction time is long, requiring 46 hours, and the conversion rate is only 75%. U.S. Patent (US 5138043) utilizes alkyl glucoside and epichlorohydrin in BF 3 Under the catalysis of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H15/04C07H1/00B01F17/56C09K23/56
Inventor 王丰收王金涛王万绪杜志平宋永波董万田
Owner SHANGHAI FINE CHEM CO LTD
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