Chromatographic column for hydrogen peroxide separation and purification

Abstract

The chromatographic column comprises a column body, an upper end sealing cover is arranged at the top of the column body, a push rod penetrates through the upper end sealing cover, the bottom of the push rod is connected with a pressing plate, a lower end sealing cover is arranged below the column body, a filter plate is arranged between the lower end sealing cover and the column body, and an opening is formed in the bottom of the lower end sealing cover and is connected with a third sealing valve body. The pressing plate can move between the upper end sealing cover and the filter plate so as to control the filling volume of the purification material, and the pressing plate is provided with a guide hole through which hydrogen peroxide can pass; the chromatographic column is made of a corrosion-resistant and oxidation-resistant high-cleanliness material, and the whole chromatographic column is connected through long threads, so that the chromatographic column has the advantages of high cleanliness, good sealing performance, high experiment accuracy and repeatability, convenience in cleaning, simplicity in operation and the like.

Description

Technical Field

[0001] The utility model relates to the field of separation and purification of hydrogen peroxide, in particular to a PFA chromatography column for separation and purification of hydrogen peroxide in a laboratory. Background Art

[0002] Hydrogen peroxide is a colorless, transparent liquid with strong oxidizing properties. It is used in pharmaceutical additives, low-temperature plasma sterilization, biosensors, pesticide additives, etc.; in the chemical industry as a new oxidant, industrial raw material, etc.; in the food industry, it is mainly used as a food additive, etc. High-purity hydrogen peroxide is obtained after purification and purification of industrial-grade hydrogen peroxide. High-purity hydrogen peroxide is one of the key basic chemical materials that are indispensable in the micro-processing and manufacturing process of electronic technology. It is mainly used as a cleaning agent, corrosive agent and photoresist remover for semiconductor crystal sheets, and in the electronics industry to prepare advanced insulating layers, remove inorganic impurities in electroplating solutions, and process copper, copper alloys and semiconductor materials gallium, germanium and cathode ray tube manufacturing processes. Its purity has a very important influence on the yield, electrical properties and reliability of integrated circuits.

[0003] For the purification of hydrogen peroxide, the membrane separation method and ion exchange resin method are currently the main methods. Regarding the ion exchange resin method, we need to complete a large amount of resin material screening in the laboratory, but the chromatography columns commonly used in the laboratory are mainly made of glass, so when they come into contact with the highly oxidizing hydrogen peroxide, some impurities will precipitate, thereby contaminating the test samples. In addition, the upper end of the column is generally open and has poor sealing. During the column process, the sample is easily contaminated by the environment, resulting in inaccurate experimental results. Utility Model Content

[0004] The utility model aims to provide a chromatography column for separation and purification of hydrogen peroxide, which has the advantages of low impurity precipitation, good stability, good sealing, easy operation and high experimental repeatability.

[0005] A chromatography column for separation and purification of hydrogen peroxide comprises a column body, an upper sealing cover is arranged on the top of the column body, a push rod passes through the upper sealing cover, the bottom of the push rod is connected to a pressing plate, a lower sealing cover is arranged below the column body, a filter plate is arranged between the lower sealing cover and the column body, and the bottom of the lower sealing cover is opened and connected to a sealing valve body.

[0006] Furthermore, a feed inlet is connected to the lower portion of the sealing valve body.

[0007] Furthermore, the outer layer of the column is provided with an interlayer, and condensation liquid can be introduced to cool the chromatography column.

[0008] Furthermore, the upper sealing cover is provided with a discharge pipe 1 and a discharge pipe 2, the discharge pipe 1 is provided with a sealing valve body 1, and the discharge pipe 2 is provided with a sealing valve body 2.

[0009] Furthermore, the pressing plate is pushed by the push rod to move between the sealing cover at the upper end of the chromatography column and the filter plate.

[0010] Furthermore, a guide hole 1 is provided on the pressing plate, the diameter of the guide hole 1 is ≤0.3 mm, and the distance between the pressing plate and the inner wall of the column is ≤0.3 mm.

[0011] Furthermore, a screw plug is provided between the push rod and the upper sealing cover, and a sealing ring is provided between the screw plug and the upper sealing cover.

[0012] Furthermore, the filter plate can be removed.

[0013] Furthermore, the column is made of tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and the upper sealing cover, lower sealing cover, push rod, pressure plate, filter plate and sealing valve body 1, sealing valve body 2 and sealing valve body 3 are made of polytetrafluoroethylene.

[0014] Furthermore, the filter plate is provided with a second guide hole, the aperture of the second guide hole is ≤0.3 mm, and the distance between the filter plate and the inner wall of the column is ≤0.3 mm.

[0015] The beneficial effects of the utility model are as follows:

[0016] (1) The chromatographic column is made of tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and the upper and lower sealing covers, push rod, pressure plate, filter plate and valve are made of polytetrafluoroethylene, which can prevent the precipitation of organic and inorganic impurities in the column during the purification and separation of hydrogen peroxide, thereby ensuring the accuracy and repeatability of the experimental results.

[0017] (2) The resin is placed between the pressure plate and the filter plate. The volume of the resin filling part can be adjusted by pushing the filter plate, thereby controlling the volume of the resin dispersed during backwashing and sample passing.

[0018] (3) The push rod, pressure plate, upper and lower sealing covers and filter plate are all removable for easy cleaning and resin loading.

[0019] (4) Two discharge pipes and a sealing valve body are provided on the sealing cover at the upper end of the chromatography column. One of the discharge pipes can be used as a pressure relief port and a sampling port. At the same time, multiple chromatography columns can be connected in series to meet the requirements of multi-stage purification of hydrogen peroxide. In addition, the sealing covers at the upper and lower ends of the chromatography column are provided with long threads, which can play a certain role in resisting pressure. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is the structural front view of the utility model.

[0021] Figure 2 It is a structural sectional view of the utility model.

[0022] Figure 3 It is a schematic diagram of the pressing plate structure of the utility model.

[0023] Figure 4 This is a schematic diagram of the filter plate structure of the utility model.

[0024] Figure 5 It is a schematic diagram of the multi-stage chromatography columns connected in series according to the utility model.

[0025] Markings in the figure: column 1, interlayer 101, guide hole 1 201, guide hole 2 202, push rod 3, screw plug 301, pressure plate 302, sealing ring 303, upper end sealing cover 4, discharge pipe 1 401, sealing valve body 1 402, discharge pipe 2 403, sealing valve body 2 404, filter plate 5, lower end sealing cover 6, sealing valve body 3 601, feed inlet 602. DETAILED DESCRIPTION

[0026] The implementation scheme of the utility model will be described in detail below in conjunction with examples. The following examples are only used to illustrate the utility model and should not be regarded as limiting the scope of the utility model.

[0027] Example 1

[0028] A chromatography column for separation and purification of hydrogen peroxide comprises a column body 1, an upper sealing cover 4 is arranged on the top of the column body 1, a push rod 3 passes through the upper sealing cover 4, the bottom of the push rod 3 is connected to a pressing plate 302, a lower sealing cover 6 is arranged below the column body 1, a filter plate 5 is arranged between the lower sealing cover 6 and the column body 1, and the bottom of the lower sealing cover 6 is opened and connected to a sealing valve body 3 601.

[0029] Furthermore, a feed inlet 602 is connected below the sealing valve body 3 601 .

[0030] Furthermore, the outer layer of the column body 1 is provided with an interlayer 101, through which condensation liquid can be introduced to cool the chromatography column.

[0031] Furthermore, the pressing plate 302 is pushed by the push rod 3 to move between the sealing cover 4 at the upper end of the chromatography column and the filter plate 5 .

[0032] Furthermore, the pressing plate 302 is provided with a conducting hole 201 , the diameter of the conducting hole 201 is ≤0.3 mm, and the distance between the pressing plate 302 and the inner wall of the column 1 is ≤0.3 mm.

[0033] Furthermore, a screw plug 301 is provided between the push rod 3 and the upper sealing cover 4 , and a sealing ring 303 is provided between the screw plug 301 and the upper sealing cover 4 .

[0034] Furthermore, the filter plate 5 can be removed.

[0035] Furthermore, the upper sealing cover 4 is provided with a discharge pipe 1 401 and a discharge pipe 2 403 . The discharge pipe 1 401 is provided with a sealing valve body 1 402 , and the discharge pipe 2 403 is provided with a sealing valve body 2 404 .

[0036] Furthermore, the filter plate 5 is provided with a second conveying hole 202 , the aperture of the second conveying hole 202 is ≤0.3 mm, and the distance between the filter plate 5 and the inner wall of the column 1 is ≤0.3 mm.

[0037] Furthermore, the column 1 is made of tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and the upper sealing cover 4, the lower sealing cover 6, the push rod 3, the pressure plate 302, the filter plate 5 and the sealing valve body 1 402, the sealing valve body 2 403, and the sealing valve body 3 601 are made of polytetrafluoroethylene.

[0038] Example 2

[0039] The device described in Example 1 is used, and the working principle is as follows: the interlayer 101 is filled with condensed water, and the separation and purification resin in the column 1 can be cooled in advance to prevent the decomposition of hydrogen peroxide during the purification and separation process. The push rod 3 is used to adjust the distance between the pressing plate 302 and the filter plate 5, and the hydrogen peroxide separation and purification resin is filled in the middle of the distance. When the distance between the pressing plate 302 and the filter plate 5 is reduced, the backwash space of the resin is reduced; when the distance between the pressing plate 302 and the filter plate 5 is increased, the backwash space of the resin is increased. For different types of resins, we can set their backwash space by controlling the distance between the pressing plate 302 and the filter plate 5. There are several guide holes 201 on the pressing plate 302, and several guide holes 202 on the filter plate 5. The apertures of the guide holes 1 201 and the guide holes 202 are both ≤0.3mm, and the distances between the filter plate 5 and the pressing plate 302 and the inner wall of the column 1 are both ≤0.3mm, which can prevent the resin particles from flowing out while passing hydrogen peroxide.

[0040] In addition, the upper sealing cover 4 and the lower sealing cover 6 are provided with long threads, which can play a certain role in resisting pressure. The lower sealing cover 6 is provided with a feed port 602, and a sealing valve body 3 601 is provided on the feed port 602. A filter plate 5 is also provided at the lower end of the column 1, and the filter plate 5 can be removed for subsequent cleaning. In addition, the push rod 3, the pressure plate 302, the lower sealing cover 6 and the upper sealing cover 4 can all be disassembled for easy cleaning and resin filling.

[0041] During operation, industrial-grade hydrogen peroxide enters the column 1 through the feed port 602, is purified by the filter plate 5 in the column 1 and the resin loaded between the pressing plate 302, and then flows out through the discharge pipe 2 403, and the discharge pipe 1 401 serves as a pressure relief port.

[0042] The upper sealing cover 4 is provided with a discharge pipe 1 401 and a discharge pipe 2 403, one of which is used as a pressure relief port and a sampling port, and the other is connected to the feed port 602 of another chromatography column, so that multiple chromatography columns can be connected in series to meet the needs of multi-stage purification of hydrogen peroxide. When conducting a multi-stage resin purification experiment, industrial-grade hydrogen peroxide is input from the feed port 602 of the chromatography column 1, and then purified by the hydrogen peroxide separation and purification resin loaded between the filter plate 5 and the pressure plate 302, and then flows out from the discharge port 403 and connected to the feed port 602 of the next chromatography column. Figure 5 As shown, at this time, the discharge port 401 can be used as a sampling port, which can facilitate graded sampling.

[0043] The above embodiments are only preferred technical solutions of the present invention and should not be regarded as limitations of the present invention. The protection scope of the present invention shall be the technical solutions recorded in the claims, including equivalent replacement solutions of the technical features in the technical solutions recorded in the claims. That is, equivalent replacement improvements within this scope are also within the protection scope of the present invention.

Claims

1. A chromatography column for separation and purification of hydrogen peroxide, characterized in that: The invention comprises a column (1), wherein an upper sealing cover (4) is provided on the top of the column (1), a push rod (3) passes through the upper sealing cover (4), the bottom of the push rod (3) is connected to a pressure plate (302), a lower sealing cover (6) is provided below the column (1), a filter plate (5) is provided between the lower sealing cover (6) and the column (1), and the bottom of the lower sealing cover (6) is open and connected to a sealing valve body (601).

2. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The sealing valve body three (601) is connected to a feed inlet (602) below.

3. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The outer layer of the column (1) is provided with an interlayer (101), through which condensation liquid can be passed to cool the chromatography column.

4. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The upper sealing cover (4) is provided with a discharge pipe 1 (401) and a discharge pipe 2 (403). The discharge pipe 1 (401) is provided with a sealing valve body 1 (402), and the discharge pipe 2 (403) is provided with a sealing valve body 2 (404).

5. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The pressing plate (302) is pushed by the push rod (3) to move between the sealing cover (4) at the upper end of the chromatography column and the filter plate (5).

6. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The pressing plate (302) is provided with a conveying hole 1 (201), the diameter of the conveying hole 1 (201) is ≤0.3 mm, and the distance between the pressing plate (302) and the inner wall of the column (1) is ≤0.3 mm.

7. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: A screw plug (301) is provided between the push rod (3) and the upper sealing cover (4), and a sealing ring (303) is provided between the screw plug (301) and the upper sealing cover (4).

8. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The filter plate (5) can be removed.

9. The chromatography column for separation and purification of hydrogen peroxide according to claim 4, characterized in that: The column (1) is made of tetrafluoroethylene-perfluoroalkoxy vinyl ether copolymer, and the upper sealing cover (4), the lower sealing cover (6), the push rod (3), the pressure plate (302), the filter plate (5) and the sealing valve body 1 (402), the sealing valve body 2 (404) and the sealing valve body 3 (601) are made of polytetrafluoroethylene.

10. The chromatography column for separation and purification of hydrogen peroxide according to claim 1, characterized in that: The filter plate (5) is provided with a second guide hole (202), the diameter of the second guide hole (202) is ≤0.3 mm, and the distance between the filter plate (5) and the inner wall of the column (1) is ≤0.3 mm.

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