KR101506309B1 - Refining apparatus of glycerin - Google Patents

Abstract

The present invention relates to a glycerin purification apparatus for preparing crude glycerin and purifying high purity glycerin using an evaporation apparatus, the apparatus comprising: a raw material tank storing the crude glycerin; A preheater connected to the raw material tank for firstly heating crude glycerin supplied from the raw material tank; A centrifugal thin film evaporator which is directly connected to the preheater and which receives heated crude glycerin and evaporates it by secondary heating, precipitates and separates foreign matters of crude glycerin and generates glycerine vapor; A pitch tank connected to the bottom of the centrifugal thin film evaporator to store foreign substances to be precipitated; A multistage condenser disposed outside the centrifugal thin film evaporator and connected to the centrifugal thin film evaporator at a lower side to receive and condense the evaporated glycerol vapor and re-discharge the unconcentrated glycerol vapor to the upper side; A recovery tank disposed below the multi-stage condenser and connected to a pipe at a lower portion of the multi-stage condenser to collect high-purity glycerin condensed in the multi-stage condenser; And a vacuum equipment connected to the multi-stage condenser to maintain the centrifugal thin film evaporator and the multi-stage condenser in a high vacuum state.
Therefore, it is possible to produce high purity glycerin which solves the purity problem of glycerin which is a disadvantage of evaporated glycerin.

Description

Refining apparatus of glycerin < RTI ID = 0.0 >

The present invention relates to an apparatus for purifying glycerin, and more particularly to an apparatus for purifying crude glycerin with high purity glycerin.

In general, the demand for glycerin is increasing because it is used for various purposes ranging from general household goods such as toothpaste and shampoo to cosmetics and medicines. Glycerin is mainly produced by refining by evaporation method, which is produced as a by-product when making fatty acids with oils or vegetable oils as a raw material or making soaps, or synthesized by using propylene as a raw material.

On the other hand, production of biodiesel has been increasing as one of the new environmentally friendly energy sources in order to suppress the increase of fossil fuel due to depletion of petroleum energy resources and the generation of carbon dioxide due to excessive use of fossil fuels. Biodiesel is produced by reacting glyceride-containing animal fats or vegetable oils with aliphatic alcohols such as methanol. In this case, glycerin is produced as a by-product together with biodiesel. When methanol is used, biodiesel is added to biodiesel Glycerin is produced at a ratio of 10: 1.

There are a variety of other methods besides the above-mentioned representative method of reacting an animal fat and vegetable oil with an aliphatic alcohol under an alkaline catalyst in a well-known method for producing biodiesel. First, animal fat and vegetable oils are reacted with aliphatic alcohols under high temperature and high pressure with an acid such as sulfuric acid as a catalyst. Second, animal fat and oil are firstly hydrolyzed to make fatty acids , A method in which the fatty acid is reacted with an aliphatic alcohol again under an acid catalyst, and a method in which an animal fat and vegetable oil are reacted with an aliphatic alcohol using an insoluble catalyst such as lanthanum oxide. Sodium methoxide is widely used as an alkali catalyst, and caustic soda and potash hydroxides are also used.

On the other hand, the trace amount of alcohol and catalyst present in the biodiesel layer is washed with water. After the washed water and the glycerin layer are combined, they are treated or neutralized with sulfuric acid or the like is generally called crude glycerin. Such crude glycerin can be used in such fields as food manufacturing pharmacy, plastic and chemical synthesis through purification. As a by-product of biodiesel, various types of crude glycerin are produced, and purification methods for crude glycerin to replace synthetic glycerin or natural purified glycerin have been actively developed.

However, since the evaporation method proceeds at a high temperature, when there is an oligomer or polymer of glycerin and an acid catalyst is used in the transesterification reaction, a small amount of various ethers formed between the alkyl alcohol and glycerin is present. Therefore, the purification of glycerin by the evaporation method is not easy to separate the pigment components present in the crude glycerin and other organic substances. Therefore, the purity of the evaporated glycerin should be increased again through activated carbon and activated carbon filtration processes.

Korean Patent Laid-Open Publication No. 10-2012-0064014 discloses an apparatus for producing a biodiesel according to an embodiment of the present invention. The apparatus for producing biodiesel according to the present invention is characterized in that a washed waste cooking oil or micro- A second agitating tank for supplying methylol and an acid catalyst to the waste edible oil or the fine algae oil for mixing the methanol and the catalyst, and a second agitating tank for mixing the methanol and the catalyst to produce methoxide, A biodiesel separation unit which is supplied with methoxide generated in the second stirring tank to produce glycerin and biodiesel, a biodiesel separation unit which evaporates and stores the biodiesel separated and transferred in the reaction tank, A glycerin separation unit for storing the glycerin after evaporating and separating foreign matters contained in the glycerin, .

However, the conventional method of purifying glycerin through the biodiesel production apparatus requires a separate filtration device according to the evaporation method, thereby increasing the production cost, and since glycerin is a by-product obtained in the process, high-purity glycerin There is still a need for glycerine purification equipment for purification.

An object of the present invention is to provide a glycerin refining apparatus for purifying crude glycerin, which is a by-product produced in the course of producing biodiesel, to separate impurities and produce high purity glycerin.

The present invention relates to a glycerin purification apparatus for preparing crude glycerin and purifying high purity glycerin using an evaporator, the apparatus comprising: a raw material tank storing the crude glycerin; A preheater connected to the raw material tank for firstly heating crude glycerin supplied from the raw material tank; A centrifugal thin film evaporator which is directly connected to the preheater and which receives heated crude glycerin and evaporates it by secondary heating, precipitates and separates foreign matters of crude glycerin and generates glycerine vapor; A pitch tank connected to the bottom of the centrifugal thin film evaporator to store foreign substances to be precipitated; A multistage condenser disposed outside the centrifugal thin film evaporator and connected to the centrifugal thin film evaporator at a lower side to receive and condense the evaporated glycerol vapor and re-discharge the unconcentrated glycerol vapor to the upper side; A recovery tank disposed below the multi-stage condenser and connected to a pipe at a lower portion of the multi-stage condenser to collect high-purity glycerin condensed in the multi-stage condenser; And a vacuum equipment connected to the multi-stage condenser to maintain the centrifugal thin film evaporator and the multi-stage condenser in a high vacuum state.

The centrifugal thin film evaporator may further include a housing having an inlet for crude glycerin supplied from a raw material tank at an upper end thereof and an outlet for evaporating and discharging crude glycerin at a lower end of the housing, The present invention relates to a process for producing glycerin, which comprises introducing a glycerin vapor into a lower portion of a mold, thereby causing the glycerin vapor to flow downward, thereby precipitating foreign substances contained in the crude glycerin and discharging the glycerin vapor through the outlet .

Also, the multi-stage condenser can continuously supply a plurality of condensers, continuously lower the temperature of the glycerol vapor supplied from the lower end of the centrifugal thin film evaporator, and cool the high-purity condensate, which is condensed through the fluid pipe provided below the multi- And then transferring the glycerin.

A flow rate sensor for detecting an inflow amount and a control unit for converting the inflow amount received from the flow rate sensor into an electrical signal; A valve that is opened or closed by a signal.

On the other hand, the recovery tank may be characterized in that a decolorizing tank is connected to the lower side, and activated carbon is filled in the decolorizing tank, and purified glycerin is added to adsorb and remove impurities.

The glycerin refining apparatus according to the present invention provides the following effects.

First, it can produce high purity glycerin which solves the purity problem of glycerin which is a disadvantage of evaporated glycerin.

Secondly, since the glycerin vapor is not lowered in the centrifugal thin film evaporator, the impurities present in the crude glycerin can be effectively removed, and in particular, the by-product such as diethyl glycol which is harmful to the human body can be easily removed have.

1 is an overall configuration diagram of a glycerin purification apparatus according to an embodiment of the present invention.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings.

BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is an overall configuration diagram of a glycerin purification apparatus according to an embodiment of the present invention; Fig.

First, referring to FIG. 1, the present invention will be described in detail. A glycerin refining apparatus according to an embodiment of the present invention can purify crude glycerin, which is a by-product generated in the production of biodiesel, to produce high purity glycerin The present invention relates to a glycerin refining apparatus comprising a raw material tank 100, a preheater 110, a centrifugal thin film evaporator 120, a pitch tank 130, a multistage condenser 140, a recovery tank 150, 160).

The raw material tank 100 stores crude glycerin and supplies the raw material to the glycerin refining apparatus 10. The raw material tank 100 is connected to the preheater 110 by piping. Further, a transfer pump may be additionally provided to supply crude glycerin to the preheater 110.

The preheater 110 is fed with crude glycerin from the raw material tank 100 and has a passage of crude glycerin therein. The preheater 110 surrounds the passage and flows through the preheater to flow heat.

The crude glycerin is firstly heated to 110 to 130 ° C in the preheater 110. The pre-heating of the crude glycerin allows sufficient heat energy to be retained in the pre-evaporation step, thereby shortening the evaporation time in the centrifugal thin film evaporator 120. If the preheating temperature is higher than the above temperature, the gasification of glycerin may occur, and if the preheating temperature is lower than the above temperature, there is not sufficient heat energy transmission effect by preheating.

The preheater 110 is connected to the centrifugal thin film evaporator to deliver crude glycerin.

The centrifugal thin film evaporator 120 includes a housing and a thin film plate. The housing has an inlet of crude glycerin supplied from the raw material tank 100 at one end thereof, and a crude glycerin vapor is evaporated at the bottom of the housing, And an outlet for discharging is formed.

The thin film plate is provided with a thin film plate which is connected to the rotating shaft at the center of the inside of the housing and is formed into a thin film by the centrifugal force of the crude glycerin which is introduced into the inside while rotating.

A heating unit (not shown) is added to the outside of the centrifugal thin film evaporator 120, and the heating unit raises the temperature of the inside of the centrifugal thin film evaporator 120 up to 290 ° C. Generally, the crude glycerin differs depending on the content of glycerin, but since vaporization starts at 165 ° C., the crude glycerin is sufficiently heated in the centrifugal thin film evaporator 120 to form glycerin vapor.

On the other hand, as the glycerin vapor is generated, the foreign substances contained in the crude glycerin are entrainment with the glycerin vapor, and the purity of the collected glycerin is lowered. Therefore, in the present invention, the thin film plate is rotated to cause foreign matter contained in the glycerin vapor to precipitate by generating a whirl.

The conventional evaporation reactor is generally configured to introduce crude glycerin into the lower portion to evaporate. The centrifugal thin film evaporator 120 supplies the crude glycerin to the upper portion of the evaporator 120, and the vacuum facility 160 The foreign substances are concentrated to the lower portion of the centrifugal thin film evaporator 120 and are easily transferred to the pitch tank 130 by the negative pressure generated by the centrifugal thin film evaporator 120. As a result, And only the glycerin vapor is discharged from the lower end of the centrifugal thin film evaporator 120.

The precipitated foreign matter is transferred to the pitch tank 130 connected to the lower side of the centrifugal thin film evaporator 120. A flow sensor 170 and a valve 180 are installed in the connection pipe between the centrifugal thin film evaporator 120 and the pitch tank 130 so that the flow sensor 170 and the valve 180 are installed in the glycerin purifier according to the amount of foreign substances precipitated in the pitch tank 130 The amount of crude glycerin can be controlled.

Meanwhile, the glycerin vapor discharged from the lower portion of the centrifugal thin film evaporator 120 is again raised along the connection pipe and supplied to the multi-stage condenser 140 disposed outside the centrifugal thin film evaporator 120.

The multi-stage condenser 140 may continuously supply a plurality of condensers, continuously lower the temperature of the glycerine vapor supplied from the lower end of the centrifugal thin film evaporator 120, The high-purity glycerin is condensed through the fluid pipe.

The glycerin vapor undergoes a stepwise cooling process in the multistage condenser 140, which is to ensure transparency of the purified glycerin. If the evaporated glycerin is cooled to room temperature once, the turbidity becomes high and it can not satisfy the usage standard for industrial use or medicine. Therefore, stepwise cooling is required to secure the transparent color of the purified glycerin.

The glycerin vapor in the multistage condenser 140 is cooled to 175 to 165 DEG C in the first condenser and to 75 to 40 DEG C in the second condenser and cooled to 45 to 30 DEG C in the third condenser. And is cooled to a room temperature of 32 캜 to 25 캜 in the fourth condenser. The cooling medium introduced at this time uses a gas according to the cooling temperature.

A pipe connecting the raw material tank 100 and the preheater 110 to the upper end of the inlet of the centrifugal thin film evaporator 120 and the pitch tank 130 are provided with a flow rate detecting unit A sensor 170, a controller (not shown) for converting an inflow amount received from the flow sensor into an electrical signal, and a valve 180 opened and closed by the electrical signal.

The recovery tank 150 is disposed below the multi-stage condenser, and is connected to a lower pipe of the multi-stage condenser 140. The glycerin vapor condensed in the multi-stage condenser 140 is transferred to and stored in the recovery tank 150, and the purity of the finally collected glycerin is 99.5% or more.

The flow sensor 170 and the valve 180 are provided in the connection pipe between the multi-stage condenser 140 and the recovery tank 150 as in the raw material tank 100, The introduction into the tank 150 can be controlled.

Further, the recovery tank may be connected to the lower side by adding a decolorizing tank (not shown). The inside of the decolorizing tank is filled with activated carbon and purified glycerin is added to adsorb and remove impurities. High-purity glycerin is purified through the multi-stage condenser 140, but transparency of glycerin can be increased when a decolorizing step is added.

In the decoloring bath, the reaction is carried out at 40 ° C to 75 ° C for 30 minutes or longer. At this time, in order to effectively discolor the glycerin can be stirred by adding a stirring device in the decoloring bath.

Meanwhile, a vacuum facility 160 is installed on one side of the multi-stage condenser 140. The vacuum equipment 160 maintains the internal air pressure of the multi-stage condenser at a high vacuum of 8 torr to 9 torr to form a negative pressure and the glycerine vapor can continuously flow from the centrifugal thin film evaporator 120 to the multi-stage condenser 140 in one direction .

Hereinafter, a process for purifying glycerin in a glycerin refining apparatus according to an embodiment of the present invention will be described with reference to the drawings.

It is preferable that crude glycerin is a by-product in the production of biodiesel and the glycerin purification apparatus 10 is installed continuously with the biodiesel production apparatus. Glycerin produced during biodiesel production is crude glycerin, which contains pigment and other organic substances, and the glycerin layer during the production of biodiesel contains excess alcohol and alkali catalyst, unreacted oil and reaction intermediates .

After the crude glycerin is separated in the biodiesel production process, it is stored in the raw material tank 100.

In the raw material tank 100, crude glycerin is pumped and introduced into the preheater 110.

In the meantime, the pre-treatment may include a step of pre-treating the pre-heater before mixing with the acid and reacting with an aliphatic alcohol by mixing with acid, preferably using hydrochloric acid (HCl).

The crude glycerin heated through the preheater 110 is supplied to the centrifugal thin film evaporator 120.

The centrifugal thin film evaporator 120 causes the generated glycerol vapor to flow downward to precipitate impurities contained in the crude glycerin and discharge the glycerin vapor through the outlet located at one side of the upper portion of the housing.

The glycerin vapor is introduced into the multi-stage condenser 140 and condensed to become pure glycerin.

The pure glycerin that has undergone the above process can be stored and transported in the recovery tank 150.

While the present invention has been described with reference to exemplary embodiments, it is to be understood that the invention is not limited to the disclosed exemplary embodiments, but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims. Accordingly, the true scope of the present invention should be determined by the technical idea of the appended claims.

10: glycerin purification apparatus 100: raw material tank
110: preheater 120: centrifugal thin film evaporator
130: Pitch tank 140: Multistage condenser
150: Recovery tank 160: Vacuum equipment
170: Flow sensor 180: Valve

Claims (5)

1. A glycerin refining apparatus for preparing crude glycerin and purifying glycerin using an evaporator,
A raw material tank for storing the crude glycerin;
A preheater connected to the raw material tank for firstly heating crude glycerin supplied from the raw material tank;
A centrifugal thin film evaporator which is directly connected to the preheater and which receives heated crude glycerin and evaporates it by secondary heating, precipitates and separates foreign matters of crude glycerin and generates glycerine vapor;
A pitch tank connected to the bottom of the centrifugal thin film evaporator to store foreign substances to be precipitated;
A multistage condenser disposed outside the centrifugal thin film evaporator and connected to the centrifugal thin film evaporator at a lower side to receive and condense the evaporated glycerol vapor and re-discharge the unconcentrated glycerol vapor to the upper side;
A recovery tank disposed below the multi-stage condenser and connected to a pipe at a lower portion of the multi-stage condenser to collect glycerin having a purity of 99.5% or more, which is condensed in the multi-stage condenser; And
And a vacuum equipment connected to the multi-stage condenser to maintain the centrifugal thin film evaporator and the multi-stage condenser in a high vacuum state. The method according to claim 1,
The centrifugal thin-
A housing formed with an inlet of crude glycerin supplied from a raw material tank at an upper end thereof and a discharge port through which a crude glycerin is evaporated and discharged at a lower end;
And a thin film plate connected to the rotating shaft at an inner center of the housing so as to be formed into a thin film by centrifugal force,
And the generated glycerin vapor is allowed to flow to the lower end to precipitate impurities contained in the crude glycerin, and the glycerin vapor is discharged through the outlet. The method according to claim 1,
The multi-
A plurality of capacitors can be installed continuously,
Wherein the temperature of the glycerin vapor supplied from one side of the lower end of the centrifugal thin film evaporator is continuously lowered and the glycerin having a purity of 99.5% or higher which is condensed through the fluid pipe provided below the multistage condenser is transferred. The method according to claim 1,
A pipe connecting the raw material tank and the preheater,
In the upper portion of the centrifugal thin film evaporator inlet and the pitch tank,
A flow rate sensor for detecting an inflow amount; a control unit for converting an inflow amount received from the flow rate sensor into an electrical signal; and a valve that is opened or closed by the electrical signal. The method according to claim 1,
Wherein the recovery tank comprises:
Wherein a decolorizing bath is added to the lower side of the decolorizing tank, and the inside of the decolorizing tank is filled with activated carbon and purified glycerin is added to adsorb and remove impurities.

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