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One-step synthesis process of dihydric alcohol amyloglycoside rosinate

A starch glycoside rosin ester and a synthesis method technology, applied in the field of surfactant synthesis, can solve the problems of long reaction process and unfavorable industrial production, and achieve the effects of fast reaction speed, excellent emulsification performance, simple equipment and operation

Inactive Publication Date: 2009-09-23
GUANGXI UNIV FOR NATITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction process is long, and measures such as vacuuming or adding water agent or nitrogen protection are required, which is not conducive to industrial production

Method used

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  • One-step synthesis process of dihydric alcohol amyloglycoside rosinate
  • One-step synthesis process of dihydric alcohol amyloglycoside rosinate
  • One-step synthesis process of dihydric alcohol amyloglycoside rosinate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Add 0.31 mole of ethylene glycol in the 250ml there-necked flask equipped with stirrer, thermometer, water separator and decompression device, 0.34 gram p-toluenesulfonic acid (accounting for 5% of rosin quality), 0.022 mole starch (calculated by glucose) and 0.021 moles of rosin, heated to 180° C. under stirring, reacted for 6 hours, and vacuum-filtered (gauge pressure 0.08-0.09 MPa) until no liquid dripped out, then stopped the suction-filtration and stopped heating. The product is cooled to room temperature, dissolved in 20ml of benzene, transferred to a 125ml separatory funnel, washed once with 10ml of 5% sodium carbonate solution, then washed three times with 10% sodium chloride solution in 40, 40, and 20ml, retaining the benzene layer and combining water box. Extract the aqueous phase with benzene three times, combine the benzene phases, distill off the solvent and recover the benzene for recycling. 9.8 grams of the product were obtained, and the conversion rate ...

Embodiment 2

[0031] Add 0.31 mol of ethylene glycol, 0.38 gram of phosphorous acid (accounting for 5% of rosin quality), 0.023 mol of starch (calculated as glucose) and 0.021 Mole rosin, under magnetic stirring, heated up to 180°C, reacted for 6 hours, and vacuum-filtered (gauge pressure 0.08-0.09MPa) until no liquid dripped out, stop the suction filtration, and stop heating. The product is cooled to room temperature, dissolved in 20ml of benzene, transferred to a 125ml separatory funnel, washed once with 10ml of 5% sodium carbonate solution, then washed three times with 10% sodium chloride solution in 40, 40, and 20ml, retaining the benzene layer and combining water box. The aqueous phase was extracted three times with benzene, the benzene phases were combined, the solvent was evaporated and the benzene was recovered for recycling. 7.1 grams of the product were obtained, and the conversion rate was 82% based on the acid value of rosin.

Embodiment 3

[0033] Add 0.31 mol of ethylene glycol, 2 ml of mixed acid (sulfuric acid: phosphoric acid = 1:3, volume ratio), 0.022 mol of starch (calculated as glucose) in a 250ml three-necked flask equipped with a stirrer, thermometer, water separator and decompression device and 0.021 moles of rosin, under magnetic stirring, heated up to 180 ° C, reacted for 6 hours, vacuum filtration (gauge pressure 0.08 ~ 0.09MPa) until no liquid dripped out, stop suction filtration, stop heating. The product is cooled to room temperature, dissolved in 20ml of benzene, transferred to a 125ml separatory funnel, washed once with 10ml of 5% sodium carbonate solution, then washed three times with 10% sodium chloride solution in 40, 40, and 20ml, retaining the benzene layer and combining water box. The aqueous phase was extracted three times with benzene, the benzene phases were combined, the solvent was evaporated and the benzene was recovered for recycling. 8.6 grams of product were obtained, and the conv...

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Abstract

The invention provides a preparation method of a nonionic surfactant, using glycol, starch and rosin as raw materials, in the presence of p-toluenesulfonic acid, phosphorous acid, phosphoric acid or mixed acids, at 180-190 ° C, turning sugar The radical reaction and the esterification reaction are carried out simultaneously to directly synthesize the diol starch glycoside rosin ester nonionic surfactant, and the conversion rate of the final product is 82-99% based on the rosin acid value. The method of the invention is simple, the reaction time is short and the conversion rate is high.

Description

technical field [0001] The invention relates to a method for synthesizing a surfactant, in particular to a method for synthesizing an oil-soluble nonionic surfactant diol starch glycoside rosin ester by using glycol, rosin and starch as raw materials. Background technique [0002] Nonionic surfactants are important raw materials for daily industrial products such as food, cosmetics, laundry detergent, shampoo, and detergent production, especially oil-soluble nonionic surfactants, which play a very important role in removing oil stains. It occupies a large proportion in washing products, but many oil-soluble nonionic surfactants currently used have the disadvantage of not being easily biodegraded, so the treatment of urban domestic sewage requires a lot of chemical or biological drugs, which increases the burden of environmental protection. Therefore, the production of "green" surfactants has become the only way for our country's daily chemical industry. [0003] Rosin and s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08B31/00C09F1/04C08K5/524
Inventor 唐世华
Owner GUANGXI UNIV FOR NATITIES
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