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Technique for preparing monoester salt of alkyl polyglucoside citric acid

A technology of alkyl polyglycoside citric acid and monoester, applied in sugar derivatives, organic chemistry, etc., can solve problems affecting product application performance, increase energy consumption, etc., achieve high monoester salt content, fast reaction speed, biological Good degradability effect

Inactive Publication Date: 2010-02-03
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent 4797481 reports the method of directly synthesizing citric acid esters with APG and citric acid as raw materials, but the reaction needs to be dehydrated at 120-140°C. In order to avoid the reactants and products from being oxidized, the reaction needs to be carried out under a nitrogen atmosphere, which improves energy efficiency. consumption
And the product produced by the direct method is a mixture of monoester salt and diester salt, the content of monoester salt is 60-80%, and the existence of diester salt affects the application performance of the product

Method used

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  • Technique for preparing monoester salt of alkyl polyglucoside citric acid
  • Technique for preparing monoester salt of alkyl polyglucoside citric acid
  • Technique for preparing monoester salt of alkyl polyglucoside citric acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] In a 250ml four-necked flask equipped with a thermometer, a stirrer, and a condenser, add 0.2mol of anhydrous citric acid and 0.2mol of propionic anhydride to mix, then heat at 40°C and react for 120min. Add 0.24mol octadecyl / decyl polyglycoside propionic acid solution into the reactor, react at 60°C for 1 hour, add squalane 1 times the volume of the reaction product, control the pressure at 35-40mmHg, and react The volatiles in the system were removed for 2 hours.

[0027] After the product was cooled, it was diluted with 200 ml of ethanol. Remove squalane, neutralize to a pH value of 9 with 50% sodium hydroxide (NaOH) aqueous solution, obtain eight / decyl polyglycoside citrate monoester disodium salt through filtration, washing, drying, product yield 95%, monoester salt content 90%.

Embodiment 2

[0029] In a 500ml four-neck flask equipped with a thermometer, agitator, and condenser, add 0.3mol of anhydrous citric acid and 0.1mol of butyric acid to mix, then add 0.9mol of butyric anhydride, heat to 100°C, and react for 15-30min . Add the dodecyl / tetradecyl polyglycoside butyric acid solution containing 0.24mol into the reactor, react at 100°C for 2 hours, add squalane twice the amount of the reaction product, and control the pressure at 5-10mmHg The reaction was carried out for 1 hour, and the volatiles in the system were removed.

[0030] After the product was cooled, dilute the reaction mixture with 300ml ethanol to remove squalane, neutralize to pH 7 with 40% potassium hydroxide (KOH) aqueous solution, obtain dodecyl / tetradecyl Polyglycoside citrate monoester dipotassium salt, the product yield is 90%, and the monoester salt content is 92%.

Embodiment 3

[0032] In a 1000ml four-necked flask equipped with a thermometer, a stirrer, and a condenser, add 0.6 mol of anhydrous citric acid and 2.4 mol of valeric acid to mix, then add 1.5 mol of valeric anhydride, and heat to 105°C for 110 minutes. Add 0.6 mol of hexadecyl / octadecanyl polyglycoside valeric acid solution into the reactor, react for a period of time at 90°C, add squalane 3 times the amount of the reaction product, and control the pressure at 5-10mmHg The reaction was carried out for 2 hours, and the volatiles in the system were removed.

[0033] After the product is cooled, dilute the reaction mixture with 300ml ethanol to remove squalane, adjust the pH value to 8 with ammonia solution, filter, wash, and dry to obtain hexadecyl / octadecanyl polyglycoside citrate monoester diammonium salt , the product yield is 95%, and the monoester salt content is 93%.

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Abstract

This invention discloses a process for preparing alkyl polyglucoside citric acid monoester. The process comprises: adding organic anhydride, organic acid and anhydrous citric acid at a mol. ratio of (1-3):(0-4):1 into a reactor, reacting at 40-110 deg.C for 15-120 min, adding alkyl polyglycoside solution, reacting at 60-110 deg.C for 1-3 h, adding dispersing medium into the reaction product, removing volatile substances under 5-40 mmHg, extracting the reaction product with a solvent, adjusting the pH value to 6-9 with an alkaline liquid, filtering, washing and drying to obtain the product. Theprocess has such advantages as low reaction temperature, rapid reaction and high monoester content.

Description

technical field [0001] The invention provides a process for preparing alkyl polyglycoside citrate monoester salt. technical background [0002] Glucose and fatty alcohol are the main raw materials, and the alkyl polyglycoside (APG) prepared after condensation has excellent surface activity, non-toxicity, and rapid and complete biodegradation. It is a typical green surfactant, but some of APG The performance is not ideal, such as the water solubility of medium and long-chain APG is not good, the foam of APG is moderate, and it decreases obviously with the increase of water hardness. In order to keep the advantages of APG and improve the disadvantages, the derivatization and modification of APG is a new topic in the study of alkyl polyglycosides. Possible derivatives of APG include non-ionic derivatives such as APG fatty acid esters, APG alkoxy derivatives; anionic derivatives such as APG sulfate, APG carboxylate salt, etc.; cationic derivatives such as APG quaternary ammoniu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H15/04C07H15/06
Inventor 杨秀全周长才
Owner CHINA RES INST OF DAILY CHEM IND