JPS5874104A - Packing method for adsorptive separating tower - Google Patents

Abstract

PURPOSE:To obtain packed beds having uniform packing structure of adsorbents and high packing density by inserting a prescribed number of oscillators into a separating tower and oscillating the same at prescribed frequencies. CONSTITUTION:Separating agents 3 are packed in an adsorptive separating tower 2. Thereafter an oscillating plate 5 transmitted with the oscillations of a vibrator 1 provided with an oscillator 4 is inserted into the separating agents and is oscillated for a specified time. The oscillator 4 is removed from the separating agents and again the agents 3 are packed. The agents 3 are packed uniformly in high packing density in the tower 2 by the repetition of such operation. In this case the number of oscillators 4 is preferably one piece in each 0.1- 100cm<2> sectional area of the separating tower, and the effect is high if frequencies are 0.1-5,000 times/sec, amplitudes are smaller than the grain sizes of the separating agents, usually 0.01-5mm. and the intensity of oscillations is smaller than the breaking strength of the separating agents.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for filling an adsorption separation column with a separation agent, and more specifically, a method for obtaining a high packing density and uniform packing structure in an adsorption separation column by using a vibrator. Minutes
The present invention relates to a method of filling an agent.

When filling an adsorption/separation tower with a separation agent, obtaining a high packing density and a uniform packing structure is a necessary condition for the adsorption/separation tower to have good separation efficiency and to maintain that efficiency over a period of time. In order to improve the separation efficiency of the adsorption separation column,
It is necessary to prevent disturbances such as tunneling of the liquid flowing inside the adsorption separation tower. To achieve this, it is necessary to create a uniform packing structure without segregation or arching of the separating agent.In order to maintain this uniform packing structure for a long period of time, it is necessary to increase the packing density of the separating agent. It is.

This is because by increasing the packing density of the separation agent, it is possible to prevent the separation agent from moving due to vibrations from outside the adsorption separation column or the pressure of the liquid, gas, or gas flow within the adsorption separation column.

However, it was extremely difficult to simultaneously add the above two conditions.

Conventionally, the hook method and the method described in Japanese Patent Publication No. 54-6990 are known as methods for filling containers with fillers. The hook method uses a hopper with a hose that extends to the surface of the filler that has settled in the filling container. Filler is poured into the hopper and hose, and the filler is removed from the bottom of the hose by slowly pulling up the hose. is how it is released. However, this method can considerably prevent filler segregation, which is one of the causes of forming a non-uniformly packed structure. However, the resulting packing density is low;
Furthermore, arching of the filler cannot be prevented at all. Further, Japanese Patent Publication No. 54-6990 discloses that according to the filling method described therein, a uniform packing structure with a high packing density of the filler can be achieved. However, adsorption separation columns require a more uniform packing structure than fixed bed reactors. This is due to the difference in the separation degree of the adsorption separation column and the means for increasing the reaction rate of the fixed bed reactor. In order to increase the reaction rate of a fixed bed reactor, the length of the fixed bed reactor in the same direction as the flow direction of the reactants is generally increased. On the other hand, in the case of an adsorption separation column, if the degree of separation is increased in the same manner as the fixed bed reactor, the recovered concentration of separated components decreases accordingly. This is a problem unique to adsorption separation columns that fixed bed reactors do not have, and is one of the reasons why adsorption separation columns require more uniform packing than fixed bed reactors.

Further, Japanese Patent Application Laid-Open No. 52-15029□4 describes a method of increasing the packing density using a vibrator.

However, increasing the packing density of fillers in this way does not necessarily result in the formation of a uniform packing structure.

Therefore, as a result of intensive research into a method of packing separation agents into an adsorption/separation tower so as to obtain a high packing density and a uniform packing structure, the present inventors have found that by inserting a vibrator into the separation tower, By vibrating under these conditions, we were able to successfully obtain a packed bed with a uniform packing structure and high packing density, and we demonstrated that an adsorption separation column using this packed bed can perform separations with extremely high separation efficiency. I found it.

The method of the present invention will be explained with reference to the accompanying drawings. First, the adsorption separation column 2 is filled with the separation agent 3. Thereafter, a diaphragm 5 to which the vibrations of the vibrator 1 including the vibrator 4 are transmitted is inserted into the separating agent and vibrated for a certain period of time. After this, the vibrator 1 is extracted from the separating agent and filled with the separating agent 3 again. This operation is repeated until the adsorption/separation column 2 is uniformly filled with 3 minutes and a high packing density. In this case, the number of vibrators is preferably one per cross-sectional area of the separation column 0, 1 to 100, and reducing the number of vibrators to less than this requires considerable technical difficulty in operating the diaphragm attached to the vibrator. It is difficult, and the effect will decrease if there are more than this.

Regarding the strength of vibration of the vibrator, if the vibrator is vibrated strongly, the separating agent will be crushed and also cause segregation. If it is weak, the arching of the separating agent cannot be broken and there is no effect. As a result of research and consideration by the inventors, the frequency is 0.
．． It has been found that it is highly effective if the vibration frequency is 1 to 5,000 times/second, the amplitude is below the particle size of the separating agent, usually 0.01 to 5 m, and the vibration strength is below the crushing strength of the separating agent. Always 1 during vibration time! 1 to 5 minutes is preferred. The vibration time is shorter than this.
If the length is too long, the effect will decrease, and if it is too long, it will cause segregation, which is not preferable. The shape of the vibrator is generally rod-like, but the effect can be expected even if it is disc-shaped.

The present invention will be explained in detail below.

Example 1 X-type zeolite (particle size 18-270 mesh) exchanged with potassium metal ions was placed in a stainless steel column with an inner diameter of 200-φ and a length of 2.5 m, and the column length was approximately 10 al.
1 was filled. After that, the vibrator was set at a frequency of 207 seconds and an amplitude of 0.
．． It was vibrated at a distance of 2 m, a vibration time of 3 minutes, and a number of vibrators of 10.0. This filling operation was repeated to fill the column with zeolite.

In order to evaluate the uniformity of the zeolite packing structure in the column thus created, the residence time distribution of this column was measured. In this measurement method, pure water is passed through the column at a constant flow rate of 8 liters/minute, and at a certain moment, potassium chloride 0.
Pulse infusions of 7 percent solution. At the column outlet, the conductivity of the liquid passing through the column was continuously measured with a conductivity needle. By measuring the electrical conductivity of the liquid distilled from the column outlet, the concentration distribution, that is, the residence time distribution, at the column outlet of the potassium chloride solution supplied to the column can be determined. The uniformity of the packing structure was evaluated based on the variance of this residence time distribution. The smaller the parance is, the more uniform the filling structure is. When calculating the parity, the starting point was the time when potassium chloride was supplied, and the value was made dimensionless by dividing by the average residence time. In this example, the parity is 1.0X10 and the packing density is 0.61g.
/m1.

Example 2 In Example 1, the frequency of the vibrator was set to 1000 times/second, and the number of vibrators was changed to 10, and the operation was performed under the same conditions as in Example 1 except for the above. As a result, the parity of the residence time distribution is 3.
0x10 and the packing density is 0.58g/mj! Met.

Example 3 The same operation as in Example 1 was performed except that activated clay (particle size range: 30 to 270 mesochets) was used. The residence time distribution parity is 1.8 x 10''~, and the packing density is 0
．． It was 50 g/mJ.

Comparative Example 1 When packing zeolite into a column, the same operation as in Example 1 was performed except that the above-mentioned sock method was used, and the variance of the residence time distribution was determined to be 5 × 10, and the packing density was It was 0.5.2 g/m1.

The parity was also large and the packing density was low.

Comparative Example 2 When filling a column with zeolite, a conical zeolite separation plate with a base diameter of 80 mm was provided at the top of the column, and zeolite was supplied from the center and filled into the column.

Other operations are the same as in the example. As a result, the packing density is 0
．． Although it was high at 57g/m#, the parity was 4X
It increased to 10.

Comparative Example 3 When the same operation as in Example 1 was performed except that the number of vibrators was changed to one in Example 1, the parity of the residence time distribution was 4.8XlO, and the packing density was 0.55 g/mj
Met. In this example, the effect of the oscillators was reduced because the number of oscillators was insufficient.

As described above, the effect of interpolating and vibrating a vibrator under certain conditions in an adsorption separation column has been clarified.

[Brief explanation of drawings]

The accompanying drawings are explanatory diagrams showing an example of an apparatus for carrying out the method of the present invention. 1... Pibre filter, 2... Adsorption separation tower, 3...
・Separating agent, 4... vibrator, 5... diaphragm. Below are blank spaces.

Claims (1)

[Claims] 1. When filling the adsorption separation tower with the separation agent, after filling the separation agent, the separation agent fixed in the adsorption separation tower is vibrated and the vibration is applied to 0.
Insert 1~100cj/piece, vibration frequency o, t~5000
A method for filling a separation agent in an adsorption separation column characterized by vibration at a rate of vibrations per second. 2. The method according to claim 1, wherein the separating agent is zeolite.