KR101970339B1 - Apparatus for producing diglycerol - Google Patents

Abstract

The present invention relates to an apparatus for producing glycidol through a dehydrocarbonation reaction using glycerol carbonate as a starting material and for producing diglycerol through a glycerol reaction with the produced glycidol, A first tank for containing glycerol carbonate; A second tank connected to the first tank through a flow path and containing at least a first solvent and a first catalyst; A third tank connected to the second tank through a flow passage for filtering and collecting the first solvent and the first catalyst used; A glycerol carbonate which is connected to the second tank through a flow path and is generated by the reaction of the glycerol carbonate with the first solvent and the first catalyst is vaporized to move along the flow path, ; And a decanter connected to the condenser and the flow path to temporarily liquefy the liquefied glycidol, wherein the decanter and the first tank are connected to each other by a flow passage, and the temporarily stored glycyrrhizene is transferred to the first tank, And the second solvent contained in the second tank and the second catalyst are reacted with each other to produce diglycerol. Therefore, a high-purity diglycerol can be produced at low cost through the reaction of glycidol and glycerin .

Description

Apparatus for producing diglycerol < RTI ID = 0.0 >

The present invention relates to an apparatus for producing diglycerol from glycerol carbonate with low cost and high purity, and more particularly, to an apparatus for producing diglycerol from glycerol carbonate using glycerol carbonate as a starting material and glycidol, , And the resulting glycidol is reacted with glycerol to produce diglycerol.

As bio-diesel technology using bio-raw materials gradually develops and interest in environmental preservation and sustainable growth grows, the market size of bio-lubricant is steadily growing.

Of the various bio-lubricating oils developed so far, the most valuable materials are diglycerol, which is conventionally produced in a state where a large amount of impurities are mixed with the conventional technology, making it difficult to separate and purify the product, and the yield is low, It is true.

Diglycerol is used directly as a cosmetic moisturizer and as a viscosity-imparting agent in shampoos. It is also used as raw material for bio lubricant (cutting oil) for lubricating performance required for metal cutting.

In addition, when at least one of the four hydroxyl groups of diglycerol is induced to esterify with a fatty acid, it can be used as a surfactant in an emulsifying agent in the food and cosmetic industry.

The condensation reaction of glycerol, which is a conventional diglycerol manufacturing process, is non-selective under acid or base catalysis, resulting in the formation of a branched dimer, cyclic diglycerol, triglycerol, tetraglycerol, etc. in addition to a linear dimer. The content of the linear dimer is less than 30%, and the existing product, diglycerol, which has a specific purity (90% or more) of the linear dimer through a multi-stage vacuum distillation process, has a high selling price.

As a technique for producing diglycerol in this way, JP-A-8-507764 " Method for producing diglycerol "

In addition, the conventional commercially available diglycerol synthesis technique is to produce diglycerol of high purity through repetitive vacuum distillation after non-selective condensation reaction of glycerol, and has a disadvantage in that the energy consumption is excessive, the purification process is expensive, .

Accordingly, the present invention has been proposed in order to overcome such problems of the prior art, and it has been proposed to optimize conditions such as reaction temperature, reaction pressure, reaction time and purity of glycidol through screening of zeolite- And to obtain diglycerol by using the resulting glycidol.

In addition, the reaction product produced during the process of producing diglycerol from glycerol can be re-introduced during the production to lower the production cost of diglycerol.

According to an aspect of the present invention for achieving the above-mentioned object, there is provided a fuel cell system comprising: a first tank containing a reaction raw material, the tank containing at least glycerol carbonate; A second tank connected to the first tank through a flow path and containing at least a first solvent and a first catalyst; A third tank connected to the second tank through a flow passage for filtering and collecting the first solvent and the first catalyst used; A glycerol carbonate which is connected to the second tank through a flow path and is generated by the reaction of the glycerol carbonate with the first solvent and the first catalyst is vaporized to move along the flow path, ; And a decanter connected to the condenser and the flow path to temporarily liquefy the liquefied glycidol, wherein the decanter and the first tank are connected to each other by a flow passage, and the temporarily stored glycyrrhizene is transferred to the first tank, And react with the second solvent and the second catalyst contained in the second tank to produce diglycerol.

In the apparatus for producing diglycerol, the second tank contains a first solvent and a first catalyst in a vacuum state at a reaction temperature of 180 ° C to 220 ° C, and the glycerol carbonate is dropped, Can be generated.

In such an apparatus for producing diglycerol, the first solvent is liquid paraffin, and the first catalyst is capable of reacting with the glycerol carbonate as a metal oxide.

The apparatus for producing diglycerol may be filled with the liquefied glycidolone temporarily stored in the decanter when the glycerol carbonate in the first tank is consumed and emptied.

When the first solvent and the first catalyst in the second tank are moved to the third tank along the flow path and emptied, the apparatus for producing diglycerol fills the second solvent and the second catalyst, glycerol and phosphoric acid , Diglycerol can be produced by allowing the glycidol of the first tank to flow and react.

As a starting material, glycerol carbonate obtained from glycerol generated from biodiesel is used as a starting material, glycidol is produced through dehydrocarbonation reaction, and then glycidol is reacted with glycerin, Diglycerol can be produced. Also, the reaction product produced during the process of producing diglycerol from glycerol can be re-introduced during the production to lower the production cost.

1 shows an apparatus for producing diglycerol according to a preferred embodiment of the present invention;

Hereinafter, embodiments of the present invention will be described in detail with reference to FIG. 1 attached hereto. The scope of the present invention will become apparent from the detailed description provided hereinafter with reference to the accompanying drawings, which are given by way of illustration only, and thus are not limitative of the present invention, and are not to be construed as limiting the present invention.

1 is a view showing an apparatus for producing diglycerol according to an embodiment of the present invention.

The apparatus for producing diglycerol comprises a first tank 100, a second tank 200, a third tank 300, a condenser 400, and a decanter 500 as a temporary storage device.

Each tank applied to the embodiment of the present invention is made of STS material with a capacity of 7 L, but the capacity and material are not limited thereto. Each tank also includes a heating means, a pressure means for applying pressure to the inside of the tank, and means for making the inside of the tank into a vacuum state.

Each of the tanks 100, 200, and 300 is provided with a case 100a, 200a, or 300a surrounding a portion of the lower portion of the tank.

In addition, in the embodiment of the present invention, the second tank 200 further includes the tilting means portion 230. Although not shown in FIG. 1, the first tank 100 and the third tank 300 may further include the tilting means 230.

The tilting means portion 230 is operated by a motor and is provided on the sides of the respective tanks 100, 200 and 300 and has an axis aligned with the center of gravity to tilt the tank.

The second tank (200) and the third tank (300) further include height adjustment parts (240, 310) capable of adjusting the height. And may be further included in the first tank 100 as needed.

The height adjusting portions 240 and 310 are pneumatic cylinders, and one or more height adjusting portions 240 and 310 are provided in each tank to adjust the height. Adjusting the height is provided for the convenience of the user to empty or fill the tank interior.

The first tank 100 is the raw material tank, and the first glycerol carbonate is accommodated. Glycerol carbonate is a glycerol carbonate obtained from glycerol generated from biodiesel using urea or the like.

The first tank 100 is connected to the second tank 200 through a raw material flow passage 101. In the embodiment of the present invention, the material flow path 101 is structurally connected below the second tank 200 to further include the pump 110.

The glycerol carbonate contained in the first tank 100 is flowed to the second tank 200 through the raw material flow passage 101 for reaction.

The second tank 200 is a reactor, in which glycerol carbonate, the first solvent and the first catalyst are reacted.

Before the glycerol carbonate is added dropwise, the first solvent and the second catalyst are filled and the reaction conditions are adjusted. At this time, the reaction conditions are set at a reaction temperature of 180 ° C to 220 ° C and a vacuum state. The solvent used is liquid paraffin having a high boiling point, and the catalyst is a metal oxide (Zn / La-based composite metal oxide) with a catalytic amount of 1 to 10 wt%.

The second tank 200 further includes a motor 210 at an upper portion thereof and an impeller 220 connected to the motor 210 is installed to stir the materials contained in the second tank 200.

The first solvent and the first catalyst accommodated in the second tank 200 react with glycerol carbonate slowly dropped to generate glycidol, which is a reaction product in the second tank 200, and is vaporized.

The glycidol produced by the reaction in the second tank 200 moves to the condenser 400 along the vaporized glycidol transfer passage 201.

The vaporized glycidol transfer passage 201 is connected to the upper part of the second tank 200 and the upper part of the condenser 400.

In an embodiment of the present invention, the condenser 400 has the following capacity.

1. Required heat exchange rate 2. Available heat exchange rate Latent heat: 233.8 kcal / kg (= 974 kJ / kg x 0.24)
Specific heat: 0.58 cal / g ℃
Specific gravity: 1.26
Boiling point: 180 ° C
Condensate liquid temperature: 40 ° C
Flow rate: 2L / 5hr

Q (5 hr) = (2 L x 1.26) x {233.8 kcal / kg + 0.58 x (180 ° C - 40 ° C)}
= 793.8 kcal
Q (1 hr avr.) = 793.8 / 5
= 158.8 kcal / hr-avr
Q (1 hr peak 1000%) = 158.8 x 10
= 1588 kcal / hr-peak Heat transfer area: 0.7 m ^ 2
Total heat transfer coefficient: 200 kcal / m ^ 2 hr ℃
Steam inlet temperature: 180 ° C
Outlet temperature: 40 ℃
Cooling water inlet temperature: 30 ℃
Coolant outlet temperature: 32 ° C

Q = 200 x 0.7 x [{(180-35) - (40-30)} / ln {(180-35) / (40-30)}]
= 7068 kcal / hr 3. Design quote Q-required = 1588 kcal / hr
Q-soluble = 7068 kcal / hr
(7068/1588) × 100 ≒ 445% compared to design

The gypsum liquefied in the condenser 400 can be condensed once in the small condenser 400a and then passed through the backflow prevention device 600. [

The small condenser 400a can be used selectively to condense and liquefy the glycidol that has not yet condensed.

The backflow prevention device 600 is composed of the exhaust gas, the condenser connecting pipe, the decanter connecting pipe, and the reactor connecting pipe (in quadrant number order) when the interior is divided into quadrants.

In addition, since a portion of the pipe connected to the reactor connection pipe is inserted into the backflow prevention device 600, the liquid level can be adjusted by the length of the pipe. When the liquid level is filled to half the level of the internal space, the steam flows toward the condenser 400.

Therefore, the backflow prevention device 600 is mounted to prevent the liquefied glycidol from returning to the second tank 200.

The backflow prevention device 600 is connected to the decanter 500 and the liquefied glycist storage flow path 401 and moves to the decanter 500 through the condenser connection pipe and the decanter connection pipe of the backflow prevention device 600. The liquefied glycidol thus moved is temporarily stored in the decanter 500.

When such a reaction is continuously performed, the first tank 100 is exhausted with all of the glycerol carbonate.

The first solvent and the second catalyst after the reaction in the second tank 200 move to the third tank 300 to empty the second tank 200. At this time, the second tank 200 is connected to the third tank 300 through the reaction material flow passage 202, and the solvent and the catalyst flow into the upper portion of the third tank 300.

In another method of emptying the second tank 200, the tilting means 230 provided on the side may be operated to tilt the second tank 200 to remove or fill the material therein.

The third tank 300 is a filtering tank, and further includes a filtering paper 310 on the upper side. Therefore, the first catalyst, which is the metal oxide moved in the second tank 200, is filtered by the filtering paper 310. In addition, the first solvent from which the first catalyst is separated is accommodated in the third tank 300 and then removed by opening the valve on the lower side (not shown).

The liquefied glycidol temporarily stored in the decanter 500 moves along the reaction channel 501 to move to the emptied first tank 100. Therefore, the first tank 100 is filled with liquefied glycidol.

)가 수용되어 100℃로, 1시간 교반함으로써 수분이 제거된다. In the second tank 200 that has been emptied, glycerol and a catalyst (phosphoric acid,

) Is accommodated and stirred at 100 DEG C for 1 hour to remove moisture.

Thereafter, the glycidol of the first tank 100 flows into the second tank 200 and is stirred at 165 DEG C for 1 hour to induce the reaction, and diglycerol is produced by such a reaction.

The diglycerol thus produced moves along the reactant flow passage 202 to the third tank 300 and is collected.

Accordingly, an apparatus for producing such diglycerol can be prepared by preparing glycerol from glycerol generated from biodiesel using glycerol carbonate obtained by using urea as a starting material, through reaction of carbon dioxide, And glycerin can be used to produce high purity diglycerol at low cost. Also, the reaction product produced during the process of producing diglycerol from glycerol can be re-introduced during the production to lower the production cost.

The apparatus for producing diglycerol according to an embodiment of the present invention as described above has been described according to the above description and drawings.

100: First tank
101: Feed flow channel
110: pump
200: Second tank
201: vaporized glycidol transfer flow path
202: (after the reaction)
210: motor
220: Im Palmer
230:
240:
300: Third tank
310: Filtering paper
320:
400: condenser
401: Liquefied glycidol storage oil
500: Decanter
501: liquefied glycidol reaction channel
600: Backflow prevention device
601: liquefied glycidol transfer path
602: Meteorological substance discharge channel

Claims (5)

A first tank (100) for containing the reaction raw material and containing at least glycerol carbonate;
A second tank (200) connected to the first tank (100) by a flow path and containing at least a first solvent and a first catalyst;
A third tank 300 connected to the second tank 200 by a flow passage for filtering and collecting the first solvent and the first catalyst used;
Glycidol generated by the reaction of the glycerol carbonate with the first solvent and the first catalyst is vaporized and connected to the second tank 200 through the flow path, A condenser 400 for liquefaction; And
And a decanter (500) connected to the condenser (400) by a flow path, wherein the liquefied glycidol is liquefied and temporarily stored,
The decanter 500 and the first tank 100 are connected to each other by a flow passage so that the temporarily stored glycyrrhythm is moved along the flow path to the first tank 100,
Reacts with the first solvent and the first catalyst contained in the second tank (200) to produce diglycerol.
The method according to claim 1,
In the second tank 200, the first solvent and the first catalyst are accommodated in a vacuum state at a reaction temperature of 180 ° C to 220 ° C, and diglycerol is produced by dropping the glycerol carbonate to produce the glycidol .
3. The method of claim 2,
Wherein the first solvent is liquid paraffin and the first catalyst is reacted with the glycerol carbonate as a metal oxide.
The method according to claim 1,
Wherein when the glycerol carbonate in the first tank (100) is consumed and emptied, the liquefied glycidol is temporarily stored in the decanter (500).
5. The method of claim 4,
When the first solvent and the first catalyst of the second tank 200 move to the third tank 300 along the flow path and are emptied, the second solvent and the second catalyst are filled with glycerol and phosphoric acid, 1 tank (100) to produce diglycerol. ≪ RTI ID = 0.0 > 8. < / RTI >

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