Method for synthetizing starch octenylsuccinate with enzymic method in ionic liquids

A technology of enzymatic synthesis of octenyl succinic acid, applied in the field of starch processing, can solve the problems of increasing the viscosity of ionic liquid and reducing the efficiency of homogeneous reaction, etc., and achieve the effect of fast reaction rate and mild reaction conditions

Active Publication Date: 2015-04-01
JIANGNAN UNIV
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Problems solved by technology

However, the introduction of long-chain hydrocarbon groups will significantly increase the

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  • Method for synthetizing starch octenylsuccinate with enzymic method in ionic liquids

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Embodiment 1

[0020] With 100mL of toluene as solvent and 0.5g of pyridine as phase transfer catalyst, add 2.5mol of sodium hydroxide, 2.5mol of deionized water, and 1.0mol of diethylene glycol monomethyl ether, then add 1.1mol of benzenesulfonyl chloride dropwise, and reflux at 70°C After 3 hours, a precipitate was formed, and the filtrate was obtained by filtration. After removing water and toluene by rotary evaporation at 70°C, it was washed with dichloromethane and water once, and the organic layer was dried by adding sodium sulfate. Finally, the dichloromethane was removed by rotary evaporation at 40°C to obtain the intermediate product 1 ( monomethyldiethyleneglycolbenzenesulfonic acid).

[0021] With 50mL of toluene as solvent and 0.5g of pyridine as phase transfer catalyst, after adding 3.0mol of sodium hydroxide, 3.0mol of deionized water, and 1.0mol of imidazole, 1.1mol of intermediate product 1 was added dropwise, refluxed at 70°C for 2h, and suction filtered to obtain Precipitat...

Embodiment 2

[0026] With 100mL toluene as solvent and 0.5g pyridine as phase transfer catalyst, add 2.5mol sodium hydroxide, 2.5mol deionized water and 1.0mol triethylene glycol monomethyl ether, then add 1.1mol benzenesulfonyl chloride dropwise, and reflux at 70°C After 3 hours, a precipitate was formed, and the filtrate was obtained by filtration. After removing water and toluene by rotary evaporation at 70°C, it was washed with dichloromethane and water once, and the organic layer was dried by adding sodium sulfate. Finally, the dichloromethane was removed by rotary evaporation at 40°C to obtain the intermediate product 1 ( monomethyltriethyleneglycolbenzenesulfonic acid).

[0027] With 50mL of toluene as the solvent and 0.5g of pyridine as the phase transfer catalyst, after adding 3.0 mol of sodium hydroxide, 3.0 mol of deionized water and 1.0 mol of imidazole, 1.1 mol of intermediate product 1 was added dropwise, refluxed at 70°C for 2 hours, and suction filtered to obtain Precipitate...

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Abstract

The invention discloses a method for synthetizing starch octenylsuccinate with an enzymic method in ionic liquids and belongs to the technical field of starch processing. The principle of the method is based on the fact that the acetic acid typeionic liquids with high cation concentration are used as efficient solvent environments for synthetizing the starch octenylsuccinate with the enzymic method, so that starch solubility is enhanced, lipase activity is kept, and the synthetizing efficiency of the starch octenylsuccinate with the enzymic method is significantly improved. According to the method, the two ionic liquids, namely, an ionic liquid 1 (Me(OEt)2-Al-Im)Ac and an ionic liquid 2 (Me(OEt)3-Al-Im)Ac, are designed and synthetized, then one of the two ionic liquids is used as a reaction solvent, 10% of common corn starch is added, subjected to pregelatinization treatment at the temperature of 100 DEG C for 10 minand cooled to the subsequent enzymic reaction temperature of 50 DEG C, octenyl succinic anhydrides accounting for 3% of the dry-basis mass of the starch and a lipase Novozym 435 accounting for 10% of the dry-basis mass of the starch are added for an esterification reaction for 30 min, a product is deposited and washed by 95% ethyl alcohol until the concentration of theanhydrides in a washing liquid is lower than 0.3%, the product is dried at the temperature of 40 DEG C and crushed, and a starch octenylsuccinate product with the substitution degree ranging from 0.014 to 0.019 is obtained.

Description

technical field [0001] The invention discloses a method for enzymatically synthesizing starch octenyl succinate in ionic liquid, relates to the application of ionic liquid in enzymatically catalyzing starch esterification, and belongs to the technical field of starch processing. Background technique [0002] Ionic liquids are non-toxic, have almost no vapor pressure, are non-volatile, have high thermal stability, can effectively dissolve a variety of organic and inorganic compounds, and have the characteristics of designability. They play an important role in chemical synthesis, especially enzymatic transformation. But at present, there are very few studies on enzymatic modification of starch in ionic liquid. This is due to the common ionic liquids that can effectively dissolve starch and other biological macromolecules, such as [bmim]Cl, in which the enzyme is usually inactive; while [bmim]BF 4 and [bmim]PF 6 Enzymatically modified benign solvents cannot dissolve starch a...

Claims

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Application Information

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IPC IPC(8): C12P19/04
CPCY02P20/54
Inventor 田耀旗李丹丹王瑞金征宇胡秀婷章宝范琴魏本喜
Owner JIANGNAN UNIV
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