Method for preparing diglyceride using bubble column reactor

Patent metadata

Field	Value
Publication number	US-10138501-B2
Application number	US-201515503226-A
Country	US
Kind code	B2
Filing date	Jul 24, 2015
Priority date	Aug 13, 2014
Publication date	Nov 27, 2018
Grant date	Nov 27, 2018

Abstract

Disclosed is a method for synthesizing diglyceride using a bubble column reactor. The method comprises the steps of: an immobilized enzyme is placed on the bearing mechanism of the bubble column reactor; a hot bath mechanism is actuated to heat the reactor body to 55-75° C.; glycerol, fatty acid and water are added into a feed chute, preheated to 55-75° C., and then transferred into the reactor body to initiate the reaction; a bubbling mechanism is actuated so that the inert gas is continuously blown into the reactor body via a sieve plate, forming boiling-like bubbles which promotes the mixing and hence to facilitate the reaction; after the reaction, the water bath mechanism and the bubbling mechanism are turned off, the heating and the inert gas circulation are stopped, a compacting mechanism is actuated, and the reaction mixture is settled and layered, thus obtaining an upper layer which is the crude glyceride layer, and a lower layer which is the glycerol layer; and the crude glyceride layer is subjected to two-stage molecular distillation so as to obtain high purity diglyceride.

First claim

The invention claimed is:

1. A method for synthesizing diglyceride using a bubble column reactor, characterized by comprising the steps of:
(1) placing an immobilized enzyme on the bearing mechanism of the bubble column reactor, and a hot bath mechanism is actuated to heat the reactor body to 55-75° C.;
(2) adding glycerol and fatty acid in a feed chute as reactants, and water is added as an activating enzyme catalyst; wherein the molar ratio of glycerol and fatty acid is 1:1-10:1; the added amount of water is less than 10% of the total mass of the reactants; and the added amount of the immobilized enzyme in step (1) is 1-10% of the total mass of the reactants;
(3) preheating glycerin, fatty acids and water in the feed chute to 55-75° C., then charged into the reactor body to initiate a synthesis reaction; a blowing mechanism is actuated and the flow rate of an inert gas is controlled at 0.7-5.7 cm/s, so that the inert gas is continuously blown into the reactor body via a sieve plate, forming boiling bubbles;
(4) turning off the hot bath mechanism and the blowing mechanism after the synthesis reaction is carried out for 15-90 min, stopping the heating and the inert gas circulation, actuating a compacting mechanism, and standing and layering the reaction mixture, thus obtaining an upper layer, which is a crude glycerin layer, and a lower layer, which is a glycerol layer; the crude glycerin layer is removed off the free fatty acids via a first-stage molecular distillation, then sent into a second-stage molecular distillation, thus obtaining a distillate and a distillation residue; wherein the distillate is high purity diglyceride, and the distillation residue is monoglyceride;
wherein the bubble column reactor in step (1) comprises a reactor body, a bearing mechanism, a sieve plate, a compacting mechanism, a blowing mechanism, a hot bath mechanism, a feed chute, and a connecting cylinder, wherein the reactor body, the bearing mechanism and the connecting cylinder are connected sequentially from top to bottom; the hot bath mechanism, the reactor body, and feed chute are sequentially connected, and formed a hot bath circulation; the reactor body is communicated with the connecting cylinder, the connecting cylinder is connected to the blowing mechanism, the sieve plate is placed on the upper end of the connecting cylinder, the compacting mechanism is mounted on the connecting cylinder, the upper end of the compacting mechanism is inserted into the connecting cylinder, and the upper end of the compacting mechanism is abutted against the sieve plate;
wherein the compacting mechanism comprises a floating joint, a cylinder, a compacting head, wherein the piston rod of the cylinder is connected to the compacting head via the floating joint, the compacting head is abutted against the sieve plate; the upper end of the compacting head is provided with a first upper cavity, the first upper cavity is communicated with the internal cavity of the reactor body via the sieve plate, the bottom surface of the first upper cavity is arranged in an inclined mode; the lower end of the compacting head is provided with a first lower cavity, the floating joint is connected to the first lower cavity; the side wall of the upper end of the compacting head is provided with a first through hole, the first through hole is communicated with the first upper cavity and the internal cavity of the connecting cylinder; and
wherein the internal cavity of the connecting cylinder is provided with flow-guiding plate, the internal cavity of the connecting cylinder is divided into a second upper cavity and the second upper cavity by the flow-guiding plate, the second upper cavity is communicated with the internal cavity of the reactor body, the flow-guiding plate is arranged in an inclined mode, the middle of the flow-guiding plate is provided with a second through hole through which the piston rod of the cylinder passes, the floating joint is sleeved with a sealing sleeve, the sealing sleeve is closely connected to the second through hole; the connecting cylinder is provided with a gas ventilating hole and a liquid collecting hole, both the gas ventilating hole and the liquid collecting hole are communicated with the second upper cavity, the gas ventilating hole is connected to the blowing mechanism; the axis of the liquid collecting hole is arranged in parallel with the flow-guiding plate, and the lower end of the flow-guiding plate is at the same height as that of the lower edge of the liquid collecting hole.

2. The method according to claim 1 , characterized in that:
the immobilized enzyme in step (1) is immobilized lipase from Candida antarctica , the added amount of the immobilized enzyme is 5% of the total mass of the reactants; and the reactor body is heated to 60° C.;
the fatty acid in step (2) is palmitic acid, oleic acid, linoleic acid, or stearic acid; the molar ratio of glycerol and fatty acid is 7.5:1; and the added amount of water is equivalent to 2.5% of the total mass of the reactants;
glycerin, fatty acid and water in the feed chute in step (3) are preheated to 60° C.; the flow rate of the inert gas is 0.83 cm/s; and the inert gas is nitrogen;
the time for the synthesis reaction in step (4) is 30 min, the time for standing and layering is 30-60 min; the first-stage molecular distillation has a distillation temperature of 150-200° C., and a pressure of 1-20 Pa, the first-stage molecular distillation has an internal condenser temperature set at 50° C., the feeds are charged continuously, the free fatty acid is distilled off, and condensed in a condenser, then enriched as a light phase by-product; the glyceride, as an undistilled heavy phase, is sent into the second-stage molecular distillation; the second-stage molecular distillation has a distillation temperature of 190-200° C. and a pressure of 0.1-5 Pa, the second-stage molecular distillation has an internal condenser temperature set at 50° C., feeds are charged continuously, the fatty acid monoglyceride is distilled off, condensed in the condenser, then collected as a light phase by-product, the heavy phase is high purity diglyceride; wherein the high purity diglyceride has a diester content of 58.46%, and a purity of ≥90%.

3. The method according to claim 1 , characterized in that the first-stage molecular distillation in step (4) has a distillation temperature of 150° C., and a pressure of 5 Pa; and the second-stage molecular distillation has a temperature of 200° C. and a pressure of 0.5 Pa.

4. The method according to claim 1 , characterized in that the blowing mechanism comprises a gas circulation booster, a condenser, a buffer tank gas, and an air compressor, wherein one end of the condenser is connected to the upper end of the reactor body, the other end of the condenser is connected to the gas circulation booster, a gas bottle for storing the inert gas is connected between the condenser and the gas circulation booster; the gas circulation booster is connected to the gas ventilating hole via the buffer tank; the air compressor is connected to the gas circulation booster, and at the same time the air compressor is connected to the cylinder.

5. The method according to claim 4 , characterized in that the hot bath is a water bath mechanism, and the water bath mechanism comprises a bathtub, a preheater, and a hot water tank, wherein the bathtub is sleeved on the reactor body, the upper end of the bathtub is connected to one end of the hot water tank via the feed chute, and the other end of the hot water tank is connected to the lower end of the bathtub via the preheater; and the buffer tank is connected to the gas ventilating hole through the preheater.

6. The method according to claim 1 , characterized in that the bearing mechanism comprises a bearing seat and a bearing cup, where

Assignees

• Univ Jinan

Inventors

• Wang Yong
• Teng Yinglai
• Liu Manman
• Zhang Ning

Classifications

• C12Y301/01003

  Triacylglycerol lipase (3.1.1.3) · CPC title

• C12P7/6454 Primary

  by esterification · CPC title

• C12P7/64

  Fats; Fatty oils; Ester-type waxes; Higher fatty acids, i.e. having at least seven carbon atoms in an unbroken chain bound to a carboxyl group; Oxidised oils or fats · CPC title

• C12M21/18

  Apparatus specially designed for the use of free, immobilized or carrier-bound enzymes · CPC title

• C12M29/08

  Air lift · CPC title