Activation and regeneration device for purification column

Abstract

The activation and regeneration device is used for activating and regenerating the purification column and comprises an activation and regeneration furnace, a plurality of connecting ports are formed in the side face of the activation and regeneration furnace, the purification column is arranged in the activation and regeneration furnace and connected with the connecting ports, the activation and regeneration furnace is connected with a nitrogen conveying pipeline, and the nitrogen conveying pipeline is communicated with the purification column. The activating and regenerating furnace is connected with a vacuumizing device, and a heating device and a temperature sensing device are arranged in the activating and regenerating furnace. The activation and regeneration device disclosed by the utility model has the beneficial effects that the activation and regeneration device can activate a newly manufactured purification column in a manner of pumping, drying and supplementing inert gas, and endows the purification column with a purification function. The residual organic solvent can be collected through liquid discharging, liquid pressing, pumping and drying and the like, and then the purification column without the organic solvent is activated, so that the purification column can be reused, one machine has two purposes, and a plurality of purification columns can be treated at one time.

Description

Technical Field

[0001] The utility model relates to the technical field of solvent purification, in particular to an activation and regeneration device for a purification column. Background Art

[0002] Organic solvents such as alcohols, ethers, benzenes, esters and halogenated hydrocarbons are commonly used in the synthesis of high-purity semiconductor materials. This type of solvent has high purity requirements and extremely low impurity content, and the price is high when used in large quantities. Therefore, costs are generally controlled by purchasing raw materials and preparing them by themselves. Before distillation, various filtering devices or purification devices are usually required to treat them to remove impurities such as water, oxygen and low-boiling substances as much as possible. The core material of these filtering or purification devices is the filter element or purification column. The filter element or purification column accessories in the prior art are generally disposable. After use, they can only be treated as solid waste because they have been soaked in various organic solvents, which not only increases semi-production costs but is also not conducive to environmental protection. There is an urgent need for a device to activate and regenerate the purification column. Utility Model Content

[0003] In order to solve the above technical problems, the utility model provides a purification column activation and regeneration device, which can not only activate the newly manufactured purification column to make it have the purification function, but also collect various organic solvents remaining in the purification column and regenerate it to have the purification function again.

[0004] Specifically, the utility model discloses a purification column activation and regeneration device, which is used for activating and regenerating the purification column, comprising: an activation regeneration furnace, a plurality of connection ports are arranged on the side of the activation regeneration furnace, the purification column is arranged in the activation regeneration furnace and connected to the connection ports, the activation regeneration furnace is connected to a nitrogen transport pipeline, the activation regeneration furnace is connected to a vacuum pumping device, and a heating device and a temperature sensing device are arranged in the activation regeneration furnace.

[0005] The benefit of adopting the above technical solution is that the activation and regeneration device can not only activate the newly manufactured purification column by means of extraction and drying and inert gas supplementation to give it purification function, but also collect the residual organic solvent by means of liquid discharge, liquid pressure, extraction and drying, and then activate the purification column after removing the organic solvent, so as to realize the reuse of the purification column, and one machine can be used for two purposes, and multiple purification columns can be processed at one time.

[0006] Furthermore, the connecting port is arranged on both sides of the activation regeneration furnace, connected with a connecting pipe, a ball valve is arranged on the connecting pipe, a plurality of the connecting pipes are connected to a manifold, the manifold is arranged on both sides of the activation regeneration furnace, and is respectively connected with an electromagnetic valve 1 and an angle valve 1.

[0007] The benefit of adopting the above technical solution is that the connecting pipes on both sides of the activation and regeneration furnace are connected to the reflux pipe to achieve the purpose of activating and regenerating multiple purification columns at one time, and the ball valves on the used pipes are opened and the unused pipes are closed.

[0008] Furthermore, the activation regeneration furnace is connected to a residual liquid containing bottle, and the residual liquid containing bottle contains liquid nitrogen.

[0009] The advantage of adopting the above technical solution is that the residual liquid holding bottle is used to collect the residual liquid in the purification column, and liquid nitrogen is provided in the residual liquid holding bottle, which can isolate air and moisture, so that the residual organic liquid can be directly used after filtering.

[0010] Furthermore, a ventilation duct is arranged above the activation regeneration furnace, an angle valve 2 is arranged on the ventilation duct, and the angle valve 1 is connected to a vacuum pumping device.

[0011] The benefit of adopting the above technical solution is that the ventilation duct is provided to introduce nitrogen into the activation regeneration furnace to ensure the activation regeneration environment, and at the same time, the activation regeneration furnace is purged to avoid overheating of the purification column.

[0012] Furthermore, the nitrogen transport pipeline is connected to branch pipeline 1 and branch pipeline 2, branch pipeline 1 is connected to solenoid valve 1, branch pipeline 2 is connected to the ventilation pipeline, flow meters are provided on branch pipeline 1 and branch pipeline 2, and solenoid valve 2 is also provided on branch pipeline 2.

[0013] The benefit of adopting the above technical solution is that the nitrogen transport pipeline transfers nitrogen to the activation regeneration furnace to supplement the inert gas for the purification column in the furnace, replace other organic solvents in the purification column, and realize the activation and regeneration of the purification column. Since different nitrogen intake amounts need to be set during activation and regeneration, the gas entering the activation regeneration furnace is controlled by a flow meter.

[0014] Furthermore, the temperature sensing device is provided in multiple locations, including a sensing device in the purification column, a middle sensing device in the furnace, a sensing device in the side wall of the furnace, and a sensing device in the outer wall of the furnace.

[0015] The advantage of adopting the above technical solution is that the temperature in the activation regeneration furnace can be accurately controlled by temperature sensing devices arranged in multiple places so as to reach the optimal temperature for activation regeneration, and at the same time, the occurrence of safety accidents can be avoided.

[0016] Furthermore, the residual liquid containing bottle is connected to a vacuum pumping component.

[0017] The advantage of adopting the above technical solution is that when removing the residual liquid, the vacuum assembly is opened, and then a vacuum environment is formed in the residual liquid container, and the residual organic solvent liquid in the purification column will enter the residual liquid container.

[0018] Furthermore, the residual liquid containing bottle is provided with an air inlet pipe and an air outlet pipe, the air inlet pipe extends into the bottom of the residual liquid containing bottle, and the air outlet pipe is connected to the vacuum pumping component.

[0019] The benefit of adopting the above technical solution is that the residual liquid extracted from the purification column directly enters the bottom of the residual liquid containing bottle, reducing the contact between the residual liquid and the air, so that the residual liquid is in a filtered state and can be used directly later.

[0020] Furthermore, a charging valve is provided at the bottom of the purification column, and an air inlet and an air outlet are provided at the top.

[0021] The advantage of adopting the above technical solution is that the purification material is added into the purification column through the bottom loading valve, and the purification column is inverted during the addition. The purification material can be one or more of 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 13X molecular sieve, lithiated molecular sieve, activated alumina, activated carbon and silica gel. BRIEF DESCRIPTION OF THE DRAWINGS

[0022] In order to more clearly illustrate the technical solutions in the embodiments of the present utility model, the drawings required to be used in the embodiments or the description of the prior art will be briefly introduced below.

[0023] Figure 1 This is a schematic diagram of the utility model for the purification column activation and regeneration device

[0024] Figure 2 This is a schematic diagram of the structure of the utility model purification column

[0025] The reference numerals in the accompanying drawings are as follows:

[0026] Activation regeneration furnace 1; connection port 11; temperature sensing device 12; connecting pipeline 13; ball valve 14; manifold 15; solenoid valve 151; angle valve 152; purification column 2; charging valve 21; air inlet 22; air outlet 23; nitrogen transport pipeline 3; branch pipeline 1 31; ball valve B131; ball valve C132 branch pipeline 2 32; flow meter 33; solenoid valve 2 34; vacuum device 4; three-way valve 41; residual liquid container 5; air inlet pipe 51; air outlet pipe 52; ventilation pipeline 6; angle valve 2 61. DETAILED DESCRIPTION

[0027] The utility model is further described in detail below in conjunction with the accompanying drawings.

[0028] like Figure 1As shown, the utility model discloses a purification column activation and regeneration device, which is used for activating and regenerating a purification column 2, comprising: an activation regeneration furnace 1, a plurality of connection ports 11 are arranged on the side of the activation regeneration furnace 1, the purification column 2 is arranged in the activation regeneration furnace 1 and connected to the connection port 11, the activation regeneration furnace 1 is connected to a nitrogen transport pipeline 3, a solenoid valve 151 is arranged between the nitrogen transport pipeline 3 and the activation regeneration furnace 1, the activation regeneration furnace 1 is connected to a vacuum pumping device 4, an angle valve 152 is arranged between the vacuum pumping device 4 and the activation regeneration furnace 1, a heating device and a temperature sensing device 12 are arranged in the activation regeneration furnace 1, the heating device can be heated by an electric heating wire, a ventilation pipe 6 is arranged above the activation regeneration furnace 1, the ventilation pipe 6 is connected to the vacuum pumping device 4 through an angle valve 61, and the vacuum pumping device 4 is connected to the angle valve 152 and the residual liquid holding bottle 5 through a three-way valve 41.

[0029] The benefit of adopting the above technical solution is that the activation and regeneration device can not only activate the newly manufactured purification column 2 by means of extraction and drying and inert gas supplementation to give it a purification function, but also collect the residual organic solvent by means of liquid discharge, liquid pressure, extraction and drying, and then activate the purification column 2 after the organic solvent is removed, so as to realize the reuse of the purification column 2, and one machine can be used for two purposes, and multiple purification columns can be processed at one time.

[0030] In some embodiments, the connecting port 11 can adopt the following structural scheme, the connecting port 11 is arranged on both sides of the activation regeneration furnace 1, and is connected to the connecting pipes 13 symmetrically arranged on both sides of the activation regeneration furnace 1, so as to achieve the purpose of activating and regenerating multiple purification columns at one time, and a ball valve 14 is arranged on the connecting pipe 13, and multiple connecting pipes 13 are connected to a manifold 15, and the manifold 15 is arranged on both sides of the activation regeneration furnace 1, and is respectively connected to the solenoid valve 151 and the angle valve 152, and the angle valve 152 is connected to a residual liquid container 5, and the residual liquid container 5 contains liquid nitrogen. The residual liquid container 5 is used to collect the residual liquid in the purification column, and liquid nitrogen is also provided in the residual liquid container 5, so that air and moisture can be isolated and the reaction of organic solvent and liquid can be avoided.

[0031] In some embodiments, the temperature sensing device 12 can adopt the following structural scheme, wherein the temperature sensing device 12 is set in multiple places, including a sensing device in the purification column 2, a middle sensing device in the furnace, a sensing device on the side wall of the furnace, and a sensing device on the outer wall of the furnace. The temperature sensing device 12 includes a temperature sensor and a display. The temperature sensor is set in the activation regeneration furnace 1 and the purification column 2, and the display is set on the outside to display the temperature value. The temperature in the activation regeneration furnace 1 can be accurately controlled by the temperature sensing devices 12 set in multiple places, so that it reaches the optimal temperature for activation and regeneration, and at the same time, the occurrence of safety accidents can be avoided.

[0032] In some embodiments, the nitrogen transport pipeline 3 can adopt the following structural scheme, the nitrogen transport pipeline 3 is connected with a branch pipeline 1 31 and a branch pipeline 2 32, the branch pipeline 1 31 is connected to the solenoid valve 1 151, the branch pipeline 2 32 is connected to the ventilation pipeline 6, the branch pipeline 1 31 and the branch pipeline 2 32 are both provided with a flow meter 33, the branch pipeline 2 32 is also provided with a solenoid valve 2 34, and the nitrogen transport pipeline 3 is connected to a nitrogen gas source.

[0033] The benefit of adopting the above technical solution is that the nitrogen transport pipeline 3 transfers nitrogen to the activation regeneration furnace 1 to supplement the inert gas for the purification column 2 in the furnace, replace other organic solvents in the purification column 2, and realize the activation and regeneration of the purification column 2. Since different nitrogen intake amounts need to be set during activation and regeneration, the gas entering the activation regeneration furnace 1 is controlled by the flow meter 33.

[0034] In some embodiments, the residual liquid container 5 may adopt the following structural scheme, wherein the residual liquid container 5 is connected to a vacuum assembly, and the residual liquid container 5 may be a Dewar liquid nitrogen bottle. When removing the residual liquid, the vacuum assembly is turned on, and then a vacuum environment is formed in the residual liquid container 5, and the residual organic solvent liquid in the purification column 2 will enter the residual liquid container 5. The residual liquid container 5 is provided with an air inlet pipe 51 and an air outlet pipe 52, wherein the air inlet pipe 51 extends into the bottom of the residual liquid container 5, and the air outlet pipe 52 is connected to the vacuum assembly.

[0035] The benefit of adopting the above technical solution is that the residual liquid extracted from the purification column 2 directly enters the bottom of the residual liquid containing bottle 5, reducing the contact between the residual liquid and the air, so that the residual liquid is in a filtered state and can be used directly later.

[0036] In some embodiments, the purification column 12 may adopt the following structural scheme, wherein a charging valve 21 is provided at the bottom of the purification column 12, a receiving cavity for receiving purification materials is provided inside, and an air inlet 22 and an air outlet 23 are provided at the top. During activation and regeneration, the air inlet 22 and the air outlet 23 are respectively connected to the activation and regeneration furnace 1, and purification materials are added to the purification column through the bottom charging valve 21. During addition, the purification column is inverted. The purification material may be one or more of 3A molecular sieve, 4A molecular sieve, 5A molecular sieve, 13X molecular sieve, lithiated molecular sieve, activated alumina, activated carbon and silica gel.

[0037] Activation process of new purification column 2: first install the purification column 2 into the furnace, connect the pipeline on the purification column 2 to the connection port 11 on both sides of the activation regeneration furnace 1 through the ferrule connection, open the ball valve B131 and ball valve C132 and angle valve 152 and angle valve 2 61 on the corresponding position connecting pipeline 13, and open the three-way valve 41 to one end of the vacuum device 4, and open the vacuum device 4. Set the flow rate of vacuuming and nitrogen filling to the purification column 2 and the activation regeneration furnace 1 through the program, set the heating to 150-300℃, and set the activation time to 12-24h. 1-12 purification columns 2 can be activated at one time.

[0038] Residual liquid recovery process: Pour out and collect the liquid in the purification column 2 after it expires, then connect it to the activation regeneration furnace 1, open the ball valve B131 and ball valve C132 and angle valve 152 and angle valve 2 61 at the corresponding positions, open the three-way valve 41 door to one side of the residual liquid bottle 5, and the vacuum assembly starts to vacuum. The flow rate of vacuuming to the purification column 12 and the activation purification furnace 1 and the flow rate ratio of nitrogen filling are set by the program, and the heating setting is set according to the physical and chemical parameters of the recovered residual liquid. At this time, the residual liquid in the purification column 2 evaporates and enters the residual liquid bottle 5, and the recovery time is set to 4 to 8 hours. The residual liquid in 1-12 purification columns 2 can be recovered at a time.

[0039] Regeneration process of purification column 2: After the residual liquid is recovered, the purification column 2 is activated again to regenerate the used purification column 2, thereby realizing the reuse of the purification column 2.

[0040] For ordinary technicians in this field, several modifications and improvements can be made without departing from the creative concept of the utility model, which all fall within the protection scope of the utility model.

Claims

1. A purification column activation and regeneration device, used for activating and regenerating a purification column (2), It is characterized in that include: An activation regeneration furnace (1), wherein a plurality of connection ports (11) are arranged on the side of the activation regeneration furnace (1), the purification column (2) is arranged in the activation regeneration furnace (1) and connected to the connection port (11), the activation regeneration furnace (1) is connected to a nitrogen transport pipeline (3), the activation regeneration furnace (1) is connected to a vacuum pumping device (4), and a heating device and a temperature sensing device (12) are arranged in the activation regeneration furnace (1).

2. The purification column activation and regeneration device according to claim 1, It is characterized in that The connection port (11) is arranged on both sides of the activation regeneration furnace (1), and is connected to a connection pipe (13), and a ball valve (14) is arranged on the connection pipe (13). A plurality of the connection pipes (13) are connected to a manifold (15), and the manifold (15) is arranged on both sides of the activation regeneration furnace (1), and is respectively connected to a solenoid valve 1 (151) and an angle valve 1 (152).

3. The purification column activation and regeneration device according to claim 1, It is characterized in that The activation regeneration furnace (1) is connected to a residual liquid storage bottle (5), and the residual liquid storage bottle (5) contains liquid nitrogen.

4. The purification column activation and regeneration device according to claim 2, It is characterized in that A ventilation duct (6) is arranged above the activation regeneration furnace (1), and a second angle valve (61) is arranged on the ventilation duct (6), and the first angle valve (152) is connected to the vacuum pump (4).

5. The purification column activation and regeneration device according to claim 4, It is characterized in that The nitrogen transport pipeline (3) is connected to a branch pipeline 1 (31) and a branch pipeline 2 (32); the branch pipeline 1 (31) is connected to the electromagnetic valve 1 (151); the branch pipeline 2 (32) is connected to the ventilation pipeline (6); flow meters (33) are provided on the branch pipeline 1 (31) and the branch pipeline 2 (32); and the branch pipeline 2 (32) is also provided with an electromagnetic valve 2 (34).

6. The purification column activation and regeneration device according to claim 1, It is characterized in that The temperature sensing device (12) is arranged in multiple places, including a sensing device in the purification column, a middle sensing device in the furnace, a sensing device on the inner side wall of the furnace, and a sensing device on the outer side wall of the furnace.

7. The purification column activation and regeneration device according to claim 3, It is characterized in that The residual liquid containing bottle (5) is connected to a vacuum pumping component.

8. The purification column activation and regeneration device according to claim 7, It is characterized in that The residual liquid containing bottle (5) is provided with an air inlet pipe (51) and an air outlet pipe (52), wherein the air inlet pipe (51) extends into the bottom of the residual liquid containing bottle (5), and the air outlet pipe (52) is connected to the vacuum pumping component.

9. The purification column activation and regeneration device according to claim 1, It is characterized in that The purification column (2) is provided with a loading valve (21) at the bottom and an air inlet (22) and an air outlet (23) at the top.

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