CN113786737A - Method for screening isotope-containing liquid separation membrane in large scale - Google Patents
Method for screening isotope-containing liquid separation membrane in large scale Download PDFInfo
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- CN113786737A CN113786737A CN202110922605.6A CN202110922605A CN113786737A CN 113786737 A CN113786737 A CN 113786737A CN 202110922605 A CN202110922605 A CN 202110922605A CN 113786737 A CN113786737 A CN 113786737A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D59/00—Separation of different isotopes of the same chemical element
- B01D59/10—Separation by diffusion
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/36—Pervaporation; Membrane distillation; Liquid permeation
- B01D61/364—Membrane distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N13/00—Investigating surface or boundary effects, e.g. wetting power; Investigating diffusion effects; Analysing materials by determining surface, boundary, or diffusion effects
- G01N2013/003—Diffusion; diffusivity between liquids
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
Abstract
The invention discloses a method for screening isotope-containing liquid separation membranes in a large scale, which solves the problems of long time consumption and high cost in screening and testing the performance of the isotope-containing liquid separation membranes in the prior art. The method for screening the isotope liquid separation membrane in a large scale comprises the steps of placing a control membrane and a plurality of membranes to be tested under the same diffusion experiment condition, inspecting the separation effect of the membranes to be tested on liquids containing different isotopes, comparing the separation effect with the separation effect of the control membrane, and inspecting the separation performance of the membranes to be tested. The control membrane is a membrane known to have separation performance in a membrane distillation separation process. The method of the invention can be used for simultaneously measuring a plurality of sample membranes under the same condition, and can quickly screen out the sample membranes meeting the requirements for the next experiment.
Description
Technical Field
The invention belongs to the technical field of nuclei, and particularly relates to a method for screening isotope-containing liquid separation membranes in a large scale.
Background
The treatment of liquids containing different isotopic elements involves a number of fields, such as the treatment of tritium (T) containing liquids in the nuclear power field (X.X.Mei, L.P.Xiong et al, Analytical Chemistry,2010,33, 201-2 18O preparation (J.K.Choi, D.S.Chang et al, Ind.Eng.chem.Res.2009,48, 5431-5438).
According to related documents (Ming Wen et al, Journal of Membrane Science,2020, 610,118237), a novel graphene hydrophobic Membrane can be prepared by a simple process, and then H is realized by combining the characteristics of Membrane distillation2O/D2O (or H)2O/HDO), and the like, similarly to H2 16O/H2 18O can also be isolated by membrane distillation according to the literature (Rasoul Moradi et al, Chemical Engineering and Processing,2016,100, 26-36). In order to prepare a high-performance separation membrane, a membrane distillation experiment needs to be performed, and the separation performance of each membrane sample prepared in the experiment is tested. It should be noted that the relevant literature (GJ Sevigny et al, Separation of treated water using graphene oxide membrane,2015) shows that heavy water (D) without radioactivity and with similar chemical properties is used2O, HDO) and tritiated Water (T)2O, HTO) are reacted with H, respectively2Because the separation results of the research on O separation have certain similarity, the research on the low tritium liquid treatment is generally carried out by using H in terms of safety, simplification problems and the like due to the radioactivity of tritium2O/D2O (or H)2O/HDO) as the subject of the study, the correlation result may be H2O/T2O (or H)2O/HTO) provides guidance.
In the prior art, the relevant literature (GJ sensing et al, Separation of treated water using a graphene oxide membrane,2015) adopts the following two methods for the performance test of the Separation membrane:
(1) under the condition of controlling the airflow, the permeation performance of the graphene film is preliminarily tested by measuring the weight loss of water vapor permeating the graphene oxide film within a certain time. Although the method can test a plurality of membrane materials simultaneously and provide certain performance test data, the time consumption is long (more than 1000 h);
(2) the other method is a method of passing a water vapor permeation experiment after high-temperature vaporization, which requires a special device and is unstable in film material.
For performance testing of separation membranes for membrane distillation applications, the current testing method can only test one membrane per experimental facility, and if a plurality of membranes need to be tested simultaneously, a plurality of sets of membrane distillation testing equipment are needed, so that the overall testing cost is high.
Therefore, a method for screening isotope liquid separation membranes on a large scale is provided, which can test the separation performance of a plurality of membranes at one time, thereby realizing short test time, high efficiency and low test cost in the process of screening the membranes, and the method becomes a problem to be solved by the technical personnel in the field.
Disclosure of Invention
The technical problem solved by the invention is as follows: provides a method for screening isotope-containing liquid separation membranes in a large scale, solves the problems that the prior art takes long time when screening and testing the performance of the isotope-containing liquid membranes,
low efficiency and high cost.
The technical scheme adopted by the invention is as follows:
the method for screening the isotope-containing liquid separation membrane in a large scale comprises the steps of placing a control membrane and a plurality of membranes to be tested under the same diffusion experiment condition, inspecting the separation effect of the membranes to be tested on the isotope-containing liquid, comparing the separation effect with the separation effect of the control membrane, and inspecting the separation performance of the membranes to be tested.
In some embodiments of the invention, the control membrane is a membrane known to have isotopic separation properties in a membrane distillation separation process.
In some embodiments of the present invention, the plurality of membranes to be tested are separated from the same isotope species or different isotope species.
Furthermore, when the isotope types separated by the membranes to be tested are different, each membrane to be tested is provided with a corresponding control membrane.
The method of the invention takes the membrane with the performance of separating the isotope in the membrane distillation separation process as the contrast, and can simultaneously test a plurality of membranes by utilizing the condition close to the membrane distillation, thereby having the advantages of rapidness and scale; the membrane structure based on the same material can be optimized; membranes of different types of materials can also be compared and membranes potentially suitable for membrane distillation processes screened.
In some embodiments of the invention, the method comprises the following steps:
s1, assembling a separation membrane and a sample bottle: covering a film to be detected on the bottleneck of the sample bottle filled with the isotope liquid, and sealing the film to be detected and the sample bottle to obtain the sample bottle covered with the film to be detected;
s2, assembling a control bottle covered with a control film according to the method of S1;
and S3, placing the sample bottle and the control bottle in a diffusion environment under the same control condition, performing a diffusion experiment, and evaluating the separation performance of the membrane covered by the sample bottle and the control bottle according to the reduced weight of the isotope liquid in the sample bottle and compared with the control bottle.
In some embodiments of the present invention, in S1, the number of sample bottles assembled on each membrane to be tested at least corresponds to the number of isotopes separated from the membrane to be tested, and each sample bottle of the membrane to be tested contains an isotope liquid. In some embodiments of the present invention, the isotope type separated by the control membrane is at least the same as that of one membrane to be tested, and the number of control bottles covered with the control membrane and the isotope liquid contained in the control bottles are the same as those of the sample bottles of the membrane to be tested.
In some embodiments of the invention, the membrane to be tested is separation H2O and D2O (or HDO) film, at least two sample bottles are assembled, wherein one or more sample bottles contain H2O, another or more sample bottles containing D2O (or HDO). Control membranes are known to separate H in membrane distillation separation processes2O and D2Films of O (or HDO); at least two are arrangedControl bottles, one or more of which contain H2O, another control bottle or bottles containing D2O (or HDO).
The membrane to be tested is separation H2O、D2O (or HDO) and T2O (or HTO) film, at least three sample bottles are provided, wherein one or more sample bottles contain H2O, another or more sample bottles containing D2O (or HDO), and the rest one or more sample bottles contain T2O (or HTO). Control membranes are known to separate H in membrane distillation separation processes2O、D2O (or HDO) and T2A film of O; at least three reference bottles are arranged, wherein one or more reference bottles contain H2O, another control bottle or a plurality of control bottles containing D2O (or HDO), and the remaining one or more control bottles contain T2O (or HTO).
In some embodiments of the present invention, in S3, the sample bottle subjected to the diffusion test and the control bottle are weighed at different time points, the weight loss ratio of the isotope liquid is calculated according to the loss amounts of different isotope liquids contained in the same membrane sample to be tested, and the calculated weight loss ratio is compared with the weight loss ratio of the corresponding control bottle to evaluate the separation performance of the membrane to be tested.
Specifically, the membrane to be tested is separation H2O and D2Film of O (or HDO), according to H contained in its sample bottle2O and D2The loss amount or average loss amount of O (or HDO) is calculated2O/D2O (or HDO) weight loss ratio, and H for control bottle2O/D2The separation performance of the membrane to be tested was evaluated by comparing the weight loss ratio of O (or HDO).
In some embodiments of the invention, the sample vial is of the same size as the control vial.
In some embodiments of the present invention, the diffusion environment for controlling conditions in S3 includes controlling vacuum degree or/and temperature.
If the isotope liquid is radioactive, the protective measures to be taken when the method of the invention is adopted should meet the relevant environmental protection and safety requirements.
Compared with the prior art, the invention has the following beneficial effects:
the invention has scientific design and ingenious conception, and can simultaneously test a plurality of film samples of different materials or/and different structures by adopting the method. The invention utilizes the similar condition of gas diffusion of the membrane distillation process, adopts the vacuumizing or heating mode to carry out the gas diffusion experiment, and can obtain the screening result in a shorter time. In addition, the membrane with the determined membrane distillation separation performance is used as a contrast, so that the separation performance of the membrane to be detected can be preliminarily determined; and can compare the separation performance of different membrane materials and membrane structures. The method effectively shortens the test time, improves the test efficiency and reduces the test cost. The method of the invention can be used for simultaneously measuring a plurality of sample membranes under the same condition, and can quickly screen out the sample membranes meeting the requirements for the next experiment.
Drawings
FIG. 1 is a schematic diagram of a testing apparatus of the present invention.
FIG. 2a is a diagram of the membrane distillation separation H of different membrane materials of example 12O/D2A separation ratio result graph of O;
FIG. 2b is a graph of H obtained by applying the process of the present invention to different membrane materials of example 12O/D2Result chart of volatilization ratio of O
FIG. 3a is a diagram of membrane distillation separation H of different membrane materials of example 22O/D2A separation ratio result graph of O; FIG. 3b is a graph of H obtained by applying the method of the present invention to different membrane materials of example 22O/D2Results of O volatilization ratio.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The present example discloses the method of the present invention for determining the separation performance of different Membrane materials, the PTFE blank Membrane with a pore size of 1 μm used in the present example is a commercially available PTFE Membrane, and the PTFE-GO composite Membrane and the PTFE-GO-PTFE composite Membrane are prepared according to the methods described in the literature (Ming Wen et al, Journal of Membrane Science,2020, 610,118237), wherein the PTFE-GO-PTFE composite Membrane is obtained by adding a layer of PTFE Membrane on the prepared PTFE-GO Membrane; membrane distillation experiments and associated separation performance calculations for these membranes were performed according to the procedures and methods described in the literature.
1. Adopting a PTFE blank membrane, a PTFE-GO composite membrane and a PTFE-GO-PTFE composite membrane to carry out membrane distillation separation of H under the same condition2O/D2The results of the O experiment are shown in FIG. 2 a: the separation ratio of the three membranes is PTFE-GO-PTFE composite membrane in sequence>PTFE-GO composite membrane>A PTFE blank membrane.
2. With the known PTFE blank membrane with separation performance in the membrane distillation separation process as a contrast, the method of the invention is used for measuring the PTFE-GO composite membrane and the PTFE-GO-PTFE composite membrane to H2O and D2Separation performance of O. The method comprises the following specific steps:
s1, assembling a separation membrane and a sample bottle: respectively contain H2O and D2And covering the bottle mouth of the O sample bottle with a PTFE-GO composite film, and sealing the O sample bottle with the sample bottle by adopting a sealing piece to obtain two sample bottles covered with the PTFE-GO composite film.
Preparing two sample bottles covered with PTFE-GO-PTFE composite membrane by the same method, wherein one sample bottle is filled with H2O, another sample bottle containing D2O。
S2, assembling a control bottle covered with a control membrane (PTFE blank membrane) according to the method of S1; assembling two control bottles, wherein one control bottle is filled with H2O, another control bottle containing D2O。
S3, placing all the sample bottles and the control bottles in the device shown in the attached drawing 1, and carrying out diffusion experiments under the condition of vacuumizing.
According to H contained in two sample bottles of the same membrane to be tested2Amount of volatilization loss of O and D2The volatilization loss of O was calculated as H2O/D2Volatilization ratio of O, and comparisonH of the bottle2O/D2And comparing the volatilization phase ratio of O, and evaluating the separation performance of the membrane to be tested. The results are shown in FIG. 2 b: the volatilization ratios of the three membranes are sequentially PTFE-GO-PTFE composite membrane>PTFE-GO composite membrane>A PTFE blank membrane.
As shown in the attached figures 2a and 2b, the PTFE-GO composite membrane and the PTFE-GO-PTFE composite membrane pair H measured by the method of the invention2O and D2The results of the separation performance of O are consistent with those obtained by adopting the membrane distillation method, which shows that the method can be used for rapidly testing the separation performance of the membrane.
Example 2
This example discloses the determination of the separation performance of different membrane materials using the method of the invention.
The PTFE blank Membrane having a pore size of 1 μm used in this example was a commercially available PTFE Membrane, and the PTFE-GO composite Membrane was prepared according to the method described in the literature (Ming Wen et al, Journal of Membrane Science,2020, 610, 118237); the PTFE-PTFE composite membrane is formed by superposing 2 PTFE blank membranes together; membrane distillation experiments and associated separation performance calculations for these membranes were performed according to the procedures and methods described in the literature.
1. Adopting a PTFE blank membrane, a PTFE-GO composite membrane and a PTFE-PTFE composite membrane to carry out membrane distillation separation of H under the same condition2O/D2The results of the O experiment are shown in FIG. 3 a: the separation ratio of the three membranes is sequentially a PTFE-PTFE composite membrane>PTFE-GO composite membrane>A PTFE blank membrane.
2. By taking a known PTFE blank membrane with separation performance in a membrane distillation separation process as a contrast, the method is adopted to determine the PTFE-GO composite membrane and the PTFE-PTFE composite membrane to H2O and D2Separation performance of O. The method comprises the following specific steps:
s1, assembling a separation membrane and a sample bottle: respectively contain H2O and D2Covering a PTFE-GO composite membrane at the bottle mouth of the O sample bottle, and sealing the O sample bottle with the sample bottle by adopting a sealing piece to obtain two sample bottles covered with the PTFE-GO composite membrane;
preparing two sample bottles covered with PTFE-PTFE composite membrane by the same method, wherein one sample bottle is filled with H2O, another sample bottle containing D2O。
S2, assembling a control bottle covered with a control membrane (PTFE blank membrane) according to the method of S1; control film two control bottles were assembled, one of which contained H2O, another control bottle containing D2O。
S3, placing all the sample bottles and the control bottles in the device shown in the attached drawing 1, and carrying out diffusion experiments under the condition of vacuumizing.
According to H contained in two sample bottles of the same membrane to be tested2Amount of volatilization loss of O and D2The volatilization loss of O was calculated as H2O/D2Volatilization ratio of O, and H of control bottle2O/D2And comparing the volatilization phase ratio of O, and evaluating the separation performance of the membrane to be tested. The results are shown in FIG. 3 b: the volatilization ratios of the three membranes are sequentially PTFE-PTFE composite membrane>PTFE-GO composite membrane>A PTFE blank membrane.
As shown in the attached figures 3a and 3b, the PTFE-GO composite membrane and the PTFE-PTFE composite membrane pair H measured by the method of the invention2O and D2The results of the separation performance of O are consistent with those obtained by adopting the membrane distillation method, which shows that the method can be used for rapidly testing the separation performance of the membrane.
In the embodiment of the invention, the isotope liquid is volatilized under the vacuum-pumping condition, and the heating condition can also be adopted to volatilize the isotope liquid. The embodiment of the invention can also achieve the technical effects by adopting heating conditions.
The embodiments described above are some, but not all embodiments of the invention. The detailed description of the embodiments of the invention is not intended to limit the scope of the invention as claimed, but merely represents selected embodiments of the invention, the precautions to be taken experimentally being in accordance with relevant environmental and safety requirements. All other embodiments obtained by a person skilled in the art without any inventive work are within the scope of protection of the present invention, based on the embodiments of the present invention and the protective measures required by the corresponding experiments.
Claims (9)
1. A method for screening separation membranes containing isotope liquid in large scale is characterized in that a control membrane and a plurality of membranes to be tested are placed under the same diffusion experiment condition, the separation effect of the membranes to be tested on the isotope liquid is inspected, and the separation effect of the membranes to be tested is compared with that of the control membrane, so that the separation performance of the membranes to be tested is inspected.
2. The method for scalably screening the isotope-containing liquid separation membrane according to claim 1, wherein the control membrane is a membrane known to have the property of separating isotopes in a membrane distillation separation process.
3. The method for screening isotope-containing liquid separation membranes in large scale according to claim 2, wherein the isotope species separated by the membranes to be tested are the same or different.
4. The method for screening isotope-containing liquid separation membranes on a large scale according to claim 3, wherein when the isotope types separated by the membranes to be tested are different, each membrane to be tested is provided with a corresponding control membrane.
5. The scalable method for screening isotope-containing liquid separation membranes according to any one of claims 1 to 4, characterized by comprising the steps of:
s1, assembling a separation membrane and a sample bottle: covering a film to be detected on the bottleneck of the sample bottle filled with the isotope liquid, and sealing the film to be detected and the sample bottle to obtain the sample bottle covered with the film to be detected;
s2, assembling a control bottle covered with a control film according to the method of S1;
and S3, placing the sample bottle and the control bottle in a diffusion environment under the same control condition, performing a diffusion experiment, and evaluating the separation performance of the membrane covered by the sample bottle and the control bottle according to the reduced weight of the isotope liquid in the sample bottle and compared with the control bottle.
6. The method for scalable screening of separation membranes for liquids containing isotopes according to claim 5, wherein in step S1, the number of sample bottles assembled on each membrane to be tested at least corresponds to the number of isotopes separated by the membrane to be tested, and each sample bottle of the membrane to be tested contains an isotope liquid.
7. The method for screening isotope-containing liquid separation membranes on a large scale according to claim 6, wherein the isotope type separated by the control membrane is at least consistent with that of one membrane to be tested, and the number of control bottles covered by the control membrane and the isotope liquid contained in the control bottles are consistent with that of a sample bottle of the membrane to be tested.
8. The method for screening separation membranes containing isotope liquids in large scale according to claim 7, wherein in S3, the weight loss ratio of isotope liquids is calculated according to the loss amount of different isotope liquids contained in the same membrane sample to be tested, and compared with the weight loss ratio of corresponding control bottles, the separation performance of the membrane to be tested is evaluated.
9. The method for scalable separation of isotope-containing liquid separation membranes according to claim 5, wherein the diffusion environment of the control condition in S3 includes controlling vacuum degree or/and temperature.
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