Microfluidic channel reactor and application thereof in synthesis of sucrose-6-palmitate

A microfluidic channel and reactor technology, applied in the direction of sugar derivatives, sugar derivatives, esterified saccharides, etc., can solve the problems of difficult separation, long reaction time, low conversion rate and selectivity, and achieve high reaction Effects of selectivity, high conversion, and shortened reaction time

Active Publication Date: 2013-07-03
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method often requires a long reaction time (24h), and the conversion rate and selectivity of the reaction are not high, and subsequent separation is difficult.

Method used

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  • Microfluidic channel reactor and application thereof in synthesis of sucrose-6-palmitate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1: Synthesis of sucrose-6-palmitate

[0030] refer to figure 1 , sucrose (0.4 mmol) was dissolved in 10 mL of tert-amyl alcohol: DMSO=4: 1 (v / v) mixed solvent, vinyl palmitate (2.0 mmol) was dissolved in 10 mL of tert-amyl alcohol, and then placed in 10 mL of spare in the syringe. 0.70g of lipase Lipozyme TLIM was evenly filled in the reaction channel of the microfluidic channel reactor. Driven by the PHD2000 syringe pump, the two-way reaction solution was injected with a total of 10.4μL·min. -1The acylation reaction was carried out through the "Y" joint at a flow rate of 100%. The temperature of the reaction channel was controlled at 52 °C by a water bath incubator, and the reaction solution flowed continuously in the reaction channel for 30 minutes. The solvent was distilled off under pressure, and the column was packed with 200-300 mesh silica gel wet method. The elution reagent was chloroform: methanol = 10: 1, the column height was 35 cm, and the column d...

Embodiment 2-5

[0034] Change the temperature of the microfluidic channel reactor, and the others are the same as in Example 1, and the reaction results are shown in Table 1:

[0035] Table 1: Effect of temperature on the reaction

[0036] Entry

[0037] The results in Table 1 show that when the flow rate is 10.4 μL·min -1 , when the reaction time is 30min, the conversion rate of the reaction increases significantly with the increase of temperature. When the reaction temperature reaches 52 °C, the conversion rate and selectivity of the reaction are the best. If the temperature continues to rise at this time, it will cause The reduction of the enzyme activity leads to a decrease in the conversion rate and selectivity of the reaction, so the optimal reaction temperature for the synthesis of sucrose-6-palmitate in the microfluidic microchannel reactor is 52 °C.

Embodiment 6-10

[0039] Change the substrate ratio of vinyl palmitate to sucrose in the microfluidic microchannel reactor to 3:1 (Example 6), 4:1 (Example 7), 6:1 (Example 8), 7:1 (Example 9), 8:1 (Example 10), the others are the same as in Example 1, and the results are shown in Table 2.

[0040] Table 2: Effect of sucrose to vinyl palmitate substrate ratio on the reaction

[0041] Example

[0042] The results in Table 2 show that with the increase of the reactant vinyl palmitate, the conversion rate of the reaction also increases. When the substrate ratio is 5:1, the conversion rate and selectivity of the reaction are the best. At this time, if the amount of the reactant vinyl palmitate continues to increase, the conversion rate and / or selectivity of the reaction will be greatly reduced. Therefore, the optimal substrate ratio of the reaction is 5:1.

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Abstract

The invention discloses a method for on-line synthesizing sucrose-6-palmitate catalyzed by a lipase. According to the method, sucrose and vinyl palmitate with a molar ratio being 1 : 3-8 are used as raw materials; 0.5-0.8 g of the lipase (Lipozyme TLIM) lipase is used as a catalyst and a mixed solvent formed by tert-amyl alcohol and DMSO is used as a reaction solvent. The lipase (Lipozyme TLIM) is uniformly filled in a reaction channel of a microfluidic channel reactor, wherein the inner diameter of the reaction channel of the microfluidic channel reactor is 0.8-2.4 mm, the length of the reaction channel is 0.5-1.0 m; the raw materials and the reaction solvent are continuously introduced into the reaction channel driven by an injection pump for an acylation reaction, wherein a temperature of the acylation reaction is controlled at 40-55 DEG C and the time of the acylation reaction is 20-40 min; a reaction liquid is collected on-line; and the sucrose-6-palmitate is obtained after the reaction liquid is subjected to conventional post-treatment. The method provided by the invention has the advantages of short reaction time, high selectivity and high yield.

Description

(1) Technical field [0001] The invention relates to a microfluidic channel reactor and its application in synthesizing sucrose-6-palmitate. (2) Background technology [0002] Microfluidics is the technology and science of manipulating nanoscale to picoliter volume fluids in micron-scale structures. It is a new interdisciplinary subject that has risen rapidly in the past decade. At present, the development of microfluidics has greatly surpassed the original purpose of serving analytical chemistry, and is becoming an important technology platform for a new round of innovative research in the entire chemistry discipline, life science, instrument science and even information science. [0003] Since Harrison's research group published the first literature on the synthesis of compounds in microfluidic chip microreactors in 1997, microfluidic chip reactors have been successfully used in a variety of organic synthesis reactions and have shown a wide range of application prospects. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J19/00C07H13/06C07H1/00
Inventor 杜理华罗锡平顾生妹张航诚胡玉婷
Owner ZHEJIANG UNIV OF TECH
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