CN214346506U

CN214346506U - Deep cleaning device for microporous resin

Info

Publication number: CN214346506U
Application number: CN202022961776.3U
Authority: CN
Inventors: 郭建宁; 付玉洁; 杨辉; 熊烨
Original assignee: Shenzhen Institute of Information Technology
Current assignee: Shenzhen Institute of Information Technology
Priority date: 2020-12-10
Filing date: 2020-12-10
Publication date: 2021-10-08
Anticipated expiration: 2030-12-10

Abstract

The utility model belongs to the technical field of the micropore resin is handled, concretely relates to micropore resin's deep washing device. The device mainly comprises a circulating pump, a cleaning column, a fixing frame and a cleaning liquid container; the middle of the cleaning column is provided with a liquid inlet 3, the liquid inlet 3 is communicated with a liquid inlet pipe 2, liquid enters the liquid inlet pipe 2 through a circulating pump 1, the lower end of the column body is provided with a G1 sand core and a liquid outlet valve 9, a liquid outlet 5 is communicated with the lower end of the column body, and the liquid is controlled to be switched on and off through the liquid outlet valve 9. The device is simple and convenient, does not need complicated equipment, can build by oneself, is applicable to the washing of most of resins, practices thrift the cost. The method for cleaning the resin by using the device is simple, can completely separate the organic solvent in the resin, improves the resin cleaning effect and ensures that the subsequent test result is more accurate. When two kinds of resin need be washd, only need add a set of mount more, wash post and pump head can, a circulating pump can be shared to two sets of devices, and the evacuation of washing liquid is direct to be accomplished through the action of gravity.

Description

Deep cleaning device for microporous resin

Technical Field

The utility model belongs to the technical field of the micropore resin is handled, concretely relates to micropore resin's deep washing device.

Background

Microporous resin is a commonly used material in industrial and chemical analysis laboratories and can be used in processes such as ion exchange, organic matter separation and the like. Since the microporous resin itself is prepared from organic materials and a large amount of organic materials remain in the micropores during the production process, the remaining materials may affect the normal use of the resin, and thus the resin is usually cleaned before use.

The conventional cleaning devices are also disclosed in related patents, but combing finds that the conventional cleaning devices are complex in structure, are mostly industrialized cleaning devices for mass production, are high in cost, are generally used for producing ion exchange resin and the like, and have the problem of insufficient cleaning, so that the conventional cleaning devices and cleaning methods are not suitable for the research needs of laboratories, because the cleanliness required by the resin used in the laboratories is far higher than that of the conventional industrial use scenes.

For solving the abluent requirement of resin under the laboratory condition, the utility model relates to a resin belt cleaning device suitable for laboratory research is fit for the deep washing of a small amount of resin, device simple structure, the method standard, can improve the abluent effect of resin with the impurity sanitization in the resin, also provide a simple and convenient device and method for research institution or water analysis laboratory simultaneously.

Disclosure of Invention

The utility model aims at providing a belt cleaning device of a small amount of resin suitable for laboratory research, it realizes through following technical scheme:

a deep cleaning device for microporous resin mainly comprises a circulating pump, a cleaning column, a fixing frame and cleaning liquid in a container; the middle of the cleaning column is provided with a liquid inlet 3, the liquid inlet 3 is communicated with a liquid inlet pipe 2, liquid enters the liquid inlet pipe 2 through a circulating pump 1, the lower end of the column body is provided with a G1 sand core and a liquid outlet valve 9, a liquid outlet 5 is communicated with the lower end of the column body, and the liquid is controlled to be switched on and off through the liquid outlet valve 9.

Preferably, the upper end of the cleaning column is designed to be a ground, the outer diameter of the upper port is 29mm, and the inner diameter of the upper port is 24 mm;

preferably, the inner diameter of the column of the cleaning column is 26mm, the outer diameter is 30mm, the effective height is 300mm, and the height-diameter ratio is 10, and the volume of the cleaning column can be enlarged or reduced according to the amount of resin to be cleaned.

The cleaning method comprises the following steps:

the cleaning solution is placed in a cleaning solution container, enters a liquid inlet pipe (as shown in figure 1) through a circulating pump, is sent into a cleaning column, can be constantly above the resin surface by adjusting the flow rate of the circulating pump and a liquid outlet valve at the lower end of the cleaning column, and is sealed by a ground glass plug, so that the liquid level is prevented from overflowing. The specific operation comprises the following steps

(1) And (5) filling resin.

The column is filled by adopting a resin wet method, the liquid level is always higher than the resin surface by 2cm in the column filling process, air bubbles are prevented from being introduced, after the resin is filled, the flow rate of a circulating pump and a liquid outlet valve at the lower end of a cleaning column are adjusted, the liquid level is constant at more than a-solidup of the resin surface, the circular immersion cleaning is realized, for the resin with lower density, a positive cleaning mode is adopted, cleaning liquid flows from top to bottom, and an upper opening of the cleaning column is sealed by a ground glass plug, so that the solution is prevented from overflowing. For the resin with higher density, a back washing mode can be adopted, and the cleaning liquid flows from bottom to top and overflows from an overflow port at the upper end.

(2) Resin cleaning

Firstly, 0.1mol/L NaOH solution with 5 times of column volume is placed in a cleaning solution container, a circulating pump is started to carry out circulating immersion cleaning for 6 hours, the solution level is kept higher than the resin level in the cleaning process, and the process is repeated for 4 times.

The pH was not changed by washing with pure water.

After emptying the pure water, putting 1.5 times of the column volume of the methanol solution into a cleaning solution container, starting a circulating pump, circularly soaking and cleaning for 6 hours, repeating the process for 4 times, emptying the solution in the cleaning column every time, discarding the soak solution, and replacing with a new methanol solution.

The column was then rinsed cyclically with 1.5 times the acetonitrile solution for 6h, the process was repeated 4 times, the soaking solution was discarded each time, and a new acetonitrile solution was replaced.

After the acetonitrile solution was drained, the column was again rinsed cyclically with 1.5 column volumes of methanol solution for 6h, the process was repeated 4 times, the solution was drained each time, the soak solution was discarded, and a new methanol solution was replaced.

And after emptying, washing the column by using pure water with 20 times of the volume of the column until the TOC of the effluent is the same as that of the pure water, closing the effluent valve after the resin is washed, taking out the resin from the upper part of the washing column, placing the resin into a glass bottle, and adding the pure water for storage for later use.

(3) Cleaning procedure before use

Before use, in order to ensure that no pollutants are dissolved out in the storage process of the resin, the resin needs to be subjected to a cleaning process before use.

First a portion of the washed resin was taken out and put into a separation column (see FIG. 2), which was rinsed through with 6 bed volumes of 0.1mol/L NaOH (Uster purity) at a flow rate not exceeding 30 bed volumes/h.

Then, the resin was washed with 6 bed volumes of pure water to remove residual alkali from the resin.

The column was then rinsed with 0.1mol/L HCl (guaranteed purity).

The resin was washed again with 6 bed volumes of purified water to remove residual acid.

This process was repeated 2 times.

And (3) using pure water to simulate a water sample to pass through the column, keeping DOC values before and after pure water passes through the column consistent, and ensuring that no organic matter is dissolved out from the resin, wherein the resin can be used at the moment. Otherwise, the cleaning process is checked, corrected and cleaned again.

The utility model discloses for prior art's beneficial effect:

(1) the device is simple and convenient, does not need complex equipment, can be built by self, is suitable for cleaning most of resins, and saves cost.

(2) The method for cleaning the resin by using the device is simple, can completely separate the organic solvent in the resin, improves the resin cleaning effect and ensures that the subsequent test result is more accurate.

(3) When two kinds of resin need be washd, only need add a set of mount more, wash post and pump head can, a circulating pump can be shared to two sets of devices, and the evacuation of washing liquid is direct to be accomplished through the action of gravity.

Drawings

Figure 1 is a diagram of an apparatus according to an embodiment of the invention. In figure 1, 1-circulating pump, 2-liquid outlet pipe, 3-liquid inlet, 4-cleaning column, 5-liquid outlet, 6-liquid inlet pipe, 7-cleaning liquid container, 8-fixing frame, 9-liquid outlet valve and 10-ground glass plug.

Fig. 2 is a diagram of an apparatus according to another embodiment of the present invention. In figure 2, 1-a fixed frame, 2-a liquid outlet pipe, 3-a separation column, 4-a circulating pump, 5-a liquid inlet pipe and 6-a cleaning liquid container.

Detailed Description

The present invention will be described in further detail with reference to the following examples and drawings, but the embodiments of the present invention are not limited thereto.

Example 1

As shown in fig. 1, a deep cleaning device for microporous resin is characterized by mainly comprising a circulating pump, a cleaning column, a fixing frame and a cleaning liquid container; the middle of the cleaning column is provided with a liquid inlet 3, the liquid inlet 3 is communicated with a liquid inlet pipe 2, liquid enters the liquid inlet pipe 2 through a circulating pump 1, the lower end of the column body is provided with a G1 sand core and a liquid outlet valve 9, a liquid outlet 5 is communicated with the lower end of the column body, and the liquid is controlled to be switched on and off through the liquid outlet valve 9.

The upper end of the cleaning column is designed as a ground, the outer diameter of the upper port is 29mm, and the inner diameter is 24 mm.

The inner diameter of the column body of the cleaning column is 26mm, the outer diameter is 30mm, the effective height is 300mm, and the height-diameter ratio is 10.

In the embodiment, the device is adopted, the resin to be cleaned is DAX-8 type resin, the resin and pure water are mixed and filled into the column by a wet method, and the liquid level is always higher than the resin by at least 2cm during the filling process of the column, so that air bubbles are prevented from being introduced. The cleaning solution is placed in a glass bottle, a circulating pump is started, a cleaning column is sealed by a glass plug, the flow of the circulating pump and a XX liquid outlet valve of the cleaning column are adjusted, and the liquid level is controlled above the resin surface to be constant. Soaking and washing for 6 hours by adopting 0.1mol/LNaOH of 5 times of column volume, repeating for four times, adjusting the liquid level to be above the resin surface, keeping constant, washing with pure water until the pH value is not changed after soaking and washing, wherein the pH value measured in the experiment is 6.43, emptying the pure water, sequentially adopting methanol (4 times) of 1.5 times of column volume, acetonitrile (4 times) of 1.5 times of column volume and methanol (4 times) of 1.5 times of column volume, emptying the soaking and washing liquid each time, washing with pure water after finishing, and ensuring that the difference between the TOC of effluent and the TOC of pure water is small, wherein the TOC values of effluent in the experiment are 0.12mg/L and 0.13mg/L, the TOC value of pure water is 0.10mg/L, the washing result is qualified, putting the washed resin into a glass bottle, and adding pure water for storage.

Before a water sample is separated by using resin, taking a part of the resin out of a glass bottle and putting the part of the resin into a separation column, filling the separation column with the height of 1/2, sequentially eluting 0.1mol/LNaOH (premium grade purity) with 6 times of bed volume, pure water with 6 times of bed volume, 0.1mol/LHCl (premium grade purity) and pure water with 6 times of bed volume through the column, repeating the process twice, simulating the column by adopting the pure water, ensuring that the DOC values before and after the pure water have very small difference, wherein the DOC values of the effluent in the experiment are 0.070mg/L and 0.078mg/L, and the effluent can pass through the column by receiving the water sample.

Example 2

In the present embodiment using the apparatus, the resin to be cleaned is XAD4 type resin in the present embodiment, and the resin is mixed with pure water and wet-packed, and the liquid level is always at least 2cm higher than the resin surface during the packing process, preventing the introduction of air bubbles. The cleaning solution is placed in a glass bottle, a circulating pump is started, a cleaning column is sealed by a glass plug, and the flow of the circulating pump and a liquid outlet valve of the cleaning column are adjusted to ensure that the liquid level is constant above the resin surface. The method comprises the steps of adopting 0.1mol/LNaOH of 5 times of column volume for immersion cleaning for 6 hours, repeating for four times, adjusting the liquid level to be constant, washing with pure water until the pH value does not change after immersion cleaning is finished, wherein the pH value measured in the experiment is 6.45, emptying the pure water, sequentially adopting methanol (4 times) of 1.5 times of column volume, acetonitrile (4 times) of 1.5 times of column volume and methanol (4 times) of 1.5 times of column volume, emptying the immersion cleaning liquid each time, washing with pure water after finishing, and enabling the difference between the TOC of effluent and the TOC of pure water to be small, wherein the TOC values of effluent in the experiment are 0.28mg/L and 0.38mg/L, the TOC value of pure water is 0.10mg/L, and the cleaning result is qualified, putting the cleaned resin into a glass bottle, and adding pure water for storage.

Before a water sample is separated by using resin, a part of the resin is taken out of a glass bottle and put into a separation column, the filling height is 1/2 of the separation column, the DOC values of the water outlet in the experiment are 0.025mg/L and 0.032mg/L, and the water outlet can receive the water sample to pass through the column, wherein the DOC values are 0.1mol/LNaOH (superior purity), 6 times of bed volume of pure water, 0.1mol/LHCl (superior purity) leaching and 6 times of bed volume of pure water leaching are sequentially carried out on the column at the position of 1/2 of the separation column, the process is repeated twice, and then the pure water is adopted to simulate the column to ensure that the difference between the DOC values before and after the pure water is very small.

Example 3

On the basis of the

embodiment

1 or 2, the cleaning program before use is further included: before use, in order to ensure that no pollutant is dissolved out in the storage process of the resin, the resin t, x, needs to be subjected to a cleaning process before use, and the cleaning process specifically comprises the following steps:

firstly, taking out a part of cleaned resin, putting the part of cleaned resin into a separation column, and leaching the part of cleaned resin through the column by using 0.1mol/L NaOH (super grade pure) with 6 times of bed volume, wherein the flow rate is not more than 30 bed volumes/h;

then washing off residual alkali liquor in the resin by using pure water with 6 times of bed volume;

then eluting the column by 0.1mol/L HCl (super pure);

washing off residual acid liquor in the resin by using pure water with 6 times of bed volume;

this process was repeated 2 times;

and (3) using pure water to simulate a water sample to pass through the column, keeping DOC values before and after pure water passes through the column consistent, and ensuring that no organic matter is dissolved out from the resin, wherein the resin can be used at the moment.

The method adopts a device as shown in figure 2, wherein, in figure 2, 1-a fixed frame, 2-a liquid outlet pipe, 3-a separation column, 4-a circulating pump, 5-a liquid inlet pipe and 6-a cleaning liquid container are adopted.

By adopting the method, the treatment effect of the resin is better.

The above embodiments are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be equivalent replacement modes, and all are included in the scope of the present invention.

Claims

1. A deep cleaning device for microporous resin is characterized by mainly comprising a circulating pump, a cleaning column, a fixing frame and a cleaning liquid container; the middle of the cleaning column is provided with a liquid inlet (3), the liquid inlet (3) is communicated with a liquid inlet pipe (2), liquid enters the liquid inlet pipe (2) through a circulating pump (1), the lower end of the column body is provided with a G1 sand core and a liquid outlet valve (9), a liquid outlet (5) is communicated with the lower end of the column body, and the liquid is controlled to be switched on and off through the liquid outlet valve (9).

2. A deep cleaning device for microporous resin according to claim 1, characterized in that the upper end of the cleaning column is preferably ground, the outer diameter of the upper end is 29mm, and the inner diameter is 24 mm.

3. A deep cleaning device for microporous resin according to claim 1, wherein the inner diameter of the column of the preferred cleaning column is 26mm, the outer diameter is 30mm, the effective height is 300mm, and the height-diameter ratio is 10.