CN113786737B - Method for large-scale screening of isotope-containing liquid separation membrane - Google Patents
Method for large-scale screening of isotope-containing liquid separation membrane Download PDFInfo
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- CN113786737B CN113786737B CN202110922605.6A CN202110922605A CN113786737B CN 113786737 B CN113786737 B CN 113786737B CN 202110922605 A CN202110922605 A CN 202110922605A CN 113786737 B CN113786737 B CN 113786737B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D59/10—Separation by diffusion
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- 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
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- B01D65/10—Testing of membranes or membrane apparatus; Detecting or repairing leaks
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- G—PHYSICS
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- 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
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- G01N2013/003—Diffusion; diffusivity between liquids
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Abstract
The invention discloses a method for large-scale screening of an isotope-containing liquid separation membrane, which solves the problems of long time consumption and high cost in screening and testing the performance of the isotope-containing liquid separation membrane in the prior art. The invention relates to a method for screening isotope liquid separation membranes in a large scale, which comprises the steps of placing a control membrane and a plurality of membranes to be tested under the same diffusion experiment condition, examining 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 examining 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 films under the same condition, and can be used for rapidly screening out sample films meeting the requirements for the next experiment.
Description
Technical Field
The invention belongs to the technical field of cores, and particularly relates to a method for screening isotope-containing liquid separation membranes in a large scale.
Background
Treatment of liquids containing different isotopic elements involves multiple fields, such as treatment of tritium (T) containing liquids in the nuclear energy field (X.X.Mei, L.P.Xiong et al Analytical Chemistry,2010,33,201-206), and H for PET in the medical industry 2 18 O preparation (J.K.Choi, D.S.Chang et al, ind. Eng. Chem. Res.2009,48, 5431-5438).
According to the related literature (Ming Wen et al Journal of Membrane Science,2020, 610,118237), a novel graphene hydrophobic membrane can be prepared by a simple process, and H can be realized by combining the characteristics of membrane distillation 2 O/D 2 O (or H) 2 O/HDO) and the like, and similarly H 2 16 O/H 2 18 O can also be separated by membrane distillation according to literature (Rasoul Moradi et al, chemical Engineering and Processing,2016,100,26-36). In order to prepare a high-performance separation membrane, an experiment of membrane distillation needs to be carried out, and separation performance of each membrane sample prepared in the experiment is tested. The relevant literature (GJ Sevigny et al, separation of tritiated water using graphene oxide membrane, 2015) shows that the use of heavy water (D) 2 O, HDO) and tritium water (T) 2 O, HTO) do separately to H 2 O separation, the separation results have a certain similarity, so that H is commonly used in research on low tritium liquid treatment in view of safety, simplification and the like due to tritium radioactivity 2 O/D 2 O (or H) 2 O/HDO) is used as a research object, and the related result can be H 2 O/T 2 O (or H) 2 O/HTO) provides guidance.
In the prior art, the performance test of the separation membrane in the related literature (GJ Sevigny et al Separation of tritiated water using graphene oxide membrane, 2015) adopts the following two methods:
(1) Under the condition of controlling air flow, the transmission performance of the graphene film is preliminarily tested by measuring the weight loss of water vapor transmitted through 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 method takes a long time (more than 1000 hours);
(2) Another method is a method of passing water vapor through experiment after vaporization at high temperature, which requires special equipment and unstable membrane material, and each experimental facility of the current test method can test only one membrane.
For performance testing of separation membranes for membrane distillation applications, the current testing method only can test one membrane per experimental facility, and if multiple membranes need to be tested simultaneously, multiple sets of membrane distillation testing equipment are needed, so that the overall cost of testing is high.
Therefore, the method for large-scale screening of the isotope liquid separation membrane can be used for testing the separation performance of a plurality of membranes at one time, so that the process of screening the membrane is short in testing time, high in efficiency and low in testing cost, and the method becomes a problem to be solved by the technicians in the field.
Disclosure of Invention
The invention solves the technical problems that: provides a method for large-scale screening of isotope-containing liquid separation membranes, which solves the problems of long time consumption during screening and testing the performance of the isotope-containing liquid separation membranes in the prior art,
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, examining 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 examining 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 invention, the isotope types of the plurality of membrane separations to be tested are the same or different.
Further, when the isotope types of the membrane to be detected are different, each membrane to be detected is provided with a corresponding control membrane.
The method of the invention takes the membrane with the isotope separation performance known in the membrane distillation separation process as a contrast, and can test a plurality of membranes simultaneously by utilizing the condition close to the membrane distillation, thereby having the advantages of rapidness and large scale; the membrane structure based on the same type of material can be optimized; membranes of different classes 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 steps of:
s1, assembling a separation membrane and a sample bottle: covering a film to be detected on the bottle mouth of the sample bottle filled with the isotope liquid, and sealing the film to be detected with 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;
s3, placing the sample bottle and the control bottle in a diffusion environment with the same control condition, performing a diffusion experiment, and evaluating the separation performance of the covered membrane according to the reduced weight of the isotope liquid in the sample bottle and comparing with the control bottle.
In some embodiments of the present invention, in S1, the number of sample bottles assembled by each of the to-be-detected films is at least equal to the number of isotope types separated by the to-be-detected film, and each sample bottle of the to-be-detected film contains one isotope liquid. In some embodiments of the present invention, the isotope types separated by the control film are at least consistent with those of one to-be-detected film, and the quantity of the control bottles covered with the control film and the isotope liquid contained in the control bottles are consistent with those of the sample bottles of the to-be-detected film.
In some embodiments of the invention, the membrane to be tested is separation H 2 O and D 2 O (or HDO) membrane, at least two sample bottles are assembled, wherein one or more sample bottles contain H 2 O, another one or more sample bottles containing D 2 O (or HDO). The control membrane is known to separate H in a membrane distillation separation process 2 O and D 2 O (or HDO) film; at least two control bottles are arranged, wherein one or more control bottles contain H 2 O, another one or more control bottles are filled with D 2 O (or HDO).
The membrane to be detected is separation H 2 O、D 2 O (or HDO) and T 2 At least three sample bottles are arranged when the membrane of O (or HTO) is arranged, wherein one or more sample bottles contain H 2 O, another one or more sample bottles containing D 2 O (or HDO), the remaining one or more sample bottles containing T 2 O (or HTO). The control membrane is known to separate H in a membrane distillation separation process 2 O、D 2 O (or HDO) and T 2 A film of O; at least three control bottles are arranged, wherein one or more control bottles contain H 2 O, another one or more control bottles are filled with D 2 O (or HDO), the remaining one or more control bottles containing T 2 O (or HTO).
In some embodiments of the present invention, in the step S3, the sample bottle and the control bottle subjected to the diffusion experiment 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 film sample to be tested, and the separation performance of the film to be tested is evaluated by comparing the weight loss ratio with the weight loss ratio of the corresponding control bottle.
Specifically, the membrane to be measured is separation H 2 O and D 2 O (or HDO) membrane, according to H contained in its sample bottle 2 O and D 2 Loss amount or average loss amount of O (or HDO), H is calculated 2 O/D 2 Weight loss ratio of O (or HDO) and H of control bottle 2 O/D 2 The weight loss ratio of O (or HDO) was compared to evaluate the separation performance of the membrane to be tested.
In some embodiments of the invention, the sample vial is the same size as the control vial.
In some embodiments of the invention, the diffusion environment of the control conditions in S3 comprises controlling vacuum or/and temperature.
If the isotope liquid has radioactivity, the protection measures to be adopted should meet the related environmental protection and safety requirements when the method is adopted.
Compared with the prior art, the invention has the following beneficial effects:
the method has scientific design and ingenious conception, and can be used for simultaneously testing a plurality of membrane samples with different materials or/and different structures. The invention uses the condition similar to the gas diffusion of the membrane distillation process, and adopts the vacuumizing or heating mode to carry out the gas diffusion experiment, thus obtaining the screening result in a shorter time. In addition, the invention uses the membrane with determined membrane distillation separation performance as a contrast, and can preliminarily determine the separation performance of the membrane to be detected; 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 films under the same condition, and can be used for rapidly screening out sample films meeting the requirements for the next experiment.
Drawings
FIG. 1 is a schematic diagram of a testing apparatus according to the present invention.
FIG. 2a shows a membrane distillation separation H of different membrane materials of example 1 2 O/D 2 A separation ratio result graph of O;
FIG. 2b is H obtained by the method of the present invention for the different membrane materials of example 1 2 O/D 2 Results of volatilization ratio of O
FIG. 3a shows a membrane distillation separation H of different membrane materials of example 2 2 O/D 2 A separation ratio result graph of O; FIG. 3b is H obtained by the method of the present invention for the different membrane materials of example 2 2 O/D 2 And O is a graph of the volatilization ratio result.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
Example 1
The present example discloses the measurement of separation performance of different membrane materials by the method of the present invention, wherein the PTFE blank membrane with a pore size of 1 μm adopted 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 method 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 to the prepared PTFE-GO membrane; membrane distillation experiments and related separation performance calculations for these membranes were carried out with reference to the processes and methods described in the literature.
1. Adopts PTFE blank membrane, PTFE-GO composite membrane and PTFE-GO-PTFE composite membrane to make membrane distillation separation H under the same condition 2 O/D 2 O experiments, results are shown in fig. 2 a: the separation ratio of the three membranes is sequentially PTFE-GO-PTFE composite membrane>PTFE-GO composite film>PTFE hollow membranes.
2. By taking a PTFE blank membrane which is known to have separation performance in a membrane distillation separation process as a comparison, the PTFE-GO composite membrane and the PTFE-GO-PTFE composite membrane pair H are measured according to the method of the invention 2 O and D 2 Separation performance of O. The method comprises the following specific steps:
s1, assembling a separation membrane and a sample bottle: respectively hold H 2 O and D 2 And covering the PTFE-GO composite film on the bottle mouth of the O sample bottle, and sealing the PTFE-GO composite film with the sample bottle by adopting a sealing piece to obtain two sample bottles covered with the PTFE-GO composite film.
Two sample bottles covered with PTFE-GO-PTFE composite film are prepared by the same method, wherein one sample bottle contains H 2 O, another sample bottle is filled with D 2 O。
S2, assembling a control bottle covered with a control film (PTFE blank film) according to the method of S1; assembling two control bottles, wherein one control bottle contains H 2 O, another control bottle is filled with D 2 O。
S3, placing all the sample bottles and the control bottles in a device shown in the attached figure 1, and performing diffusion experiments under the condition of vacuumizing.
H contained in two sample bottles according to the same film to be tested 2 Amount of volatilization loss of O and D 2 O volatilization loss amount, calculating H 2 O/D 2 Volatilizing ratio of O and H of the reference bottle 2 O/D 2 And (3) comparing the volatilization ratio of O, and evaluating the separation performance of the film to be tested. The results are shown in FIG. 2 b: the volatilization ratio of the three membranes is sequentially PTFE-GO-PTFE composite membrane>PTFE-GO composite film>PTFEAnd (5) blank films.
As can be seen from fig. 2a and 2b, the PTFE-GO composite membrane and the PTFE-GO-PTFE composite membrane pair H measured by the method of the present invention 2 O and D 2 The results of the separation performance of O are consistent with those obtained by adopting a 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 measurement of the separation performance of different membrane materials using the method of the present invention.
The 1 μm pore size PTFE blank membrane 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 film is formed by superposing 2 PTFE blank films together; membrane distillation experiments and related separation performance calculations for these membranes were carried out with reference to the processes and methods described in the literature.
1. Adopts PTFE blank membrane, PTFE-GO composite membrane and PTFE-PTFE composite membrane to make membrane distillation separation H under the same condition 2 O/D 2 O experiments, results are shown in fig. 3 a: the separation ratio of the three membranes is PTFE-PTFE composite membrane>PTFE-GO composite film>PTFE hollow membranes.
2. By taking a PTFE blank membrane which is known to have separation performance in a membrane distillation separation process as a comparison, the method is adopted to determine the PTFE-GO composite membrane and the pair H of the PTFE-PTFE composite membrane 2 O and D 2 Separation performance of O. The method comprises the following specific steps:
s1, assembling a separation membrane and a sample bottle: respectively hold H 2 O and D 2 Covering a PTFE-GO composite film on the bottleneck of the sample bottle of O, and sealing the sample bottle with the PTFE-GO composite film by adopting a sealing piece to obtain two sample bottles covered with the PTFE-GO composite film;
two sample bottles covered with PTFE-PTFE composite film are prepared by the same method, wherein one sample bottle contains H 2 O, another sample bottle is filled with D 2 O。
S2, assembling a control bottle covered with a control film (PTFE blank film) according to the method of S1; the control film is assembled into two control bottles, wherein one control bottle contains H 2 O, anotherControl bottle contains D 2 O。
S3, placing all the sample bottles and the control bottles in a device shown in the attached figure 1, and performing diffusion experiments under the condition of vacuumizing.
H contained in two sample bottles according to the same film to be tested 2 Amount of volatilization loss of O and D 2 O volatilization loss amount, calculating H 2 O/D 2 Volatilizing ratio of O and H of the reference bottle 2 O/D 2 And (3) comparing the volatilization ratio of O, and evaluating the separation performance of the film to be tested. The results are shown in FIG. 3 b: the volatilization ratio of the three membranes is PTFE-PTFE composite membrane>PTFE-GO composite film>PTFE hollow membranes.
As can be seen from FIGS. 3a and 3b, the PTFE-GO composite membrane and the PTFE-PTFE composite membrane pair H measured by the method of the present invention 2 O and D 2 The results of the separation performance of O are consistent with those obtained by adopting a 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 vacuumizing condition, and the isotope liquid can be volatilized under the heating condition. The embodiment of the invention can also realize 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 is merely representative of selected embodiments of the invention, as the protective measures that the experiment needs to take should meet the relevant environmental and safety requirements. All other embodiments, which can be made by a person of ordinary skill in the art without any inventive effort, are within the scope of the present invention based on the embodiments of the present invention and the protective measures that the corresponding experiments need to take.
Claims (6)
1. A method for screening isotope-containing liquid separation membranes in a large scale is characterized by comprising the steps of placing a control membrane and a plurality of membranes to be tested under the same diffusion experiment condition, examining 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 examining the separation performance of the membranes to be tested; the control membrane is a membrane known to have isotope separation performance in a membrane distillation separation process;
the method comprises the following steps:
s1, assembling a separation membrane and a sample bottle: covering a film to be detected on the bottle mouth of the sample bottle filled with the isotope liquid, and sealing the film to be detected with 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;
s3, placing the sample bottle and the control bottle in a diffusion environment with the same control condition, performing a diffusion experiment, and evaluating the separation performance of a film covered by the sample bottle and the control bottle according to the reduced weight of the isotope liquid in the sample bottle;
the diffusion environment of the control condition in S3 includes controlling the vacuum degree or/and the temperature.
2. The method for large-scale screening of isotopic liquid separation membranes according to claim 1, wherein the isotopic species of the plurality of membrane separations to be tested are the same or different.
3. The method for large-scale screening of isotopic liquid separation membranes according to claim 2, wherein when the isotopic species separated by the membranes to be tested are different, each membrane to be tested is provided with a corresponding control membrane.
4. The method for large-scale screening of isotopic liquid separation membranes according to claim 1, wherein in S1, the number of sample bottles assembled for each membrane to be tested is at least equal to the number of isotopic species separated for the membrane to be tested, and each sample bottle of the membrane to be tested contains an isotopic liquid.
5. The method of claim 4, wherein the isotope type of the control membrane is at least consistent with that of one membrane to be tested, and the number of control bottles covering the control membrane and the isotope liquid contained in the control bottles are consistent with that of the sample bottles of the membrane to be tested.
6. The method for large-scale screening of separation membranes for liquids containing isotopes according to claim 5, wherein in S3, the weight loss ratio of the isotopic liquid is calculated according to the loss amounts of different isotopic liquids contained in the same sample of the membrane to be tested, and compared with the weight loss ratio of the corresponding control bottle, the separation performance of the membrane to be tested is evaluated.
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Appropriate coating pretreatment enhancing osmotic dehydration efficiency of scallop adductors;Tian Yuan等;农业工程学报;第32卷(第17期);266-273 * |
PEBA/MCM-41杂化膜的制备及其对苯酚/水渗透汽化分离性能的研究;王敏敏;张新儒;李馨然;郝晓刚;李春成;丁川;王倩;;膜科学与技术(第06期);44-51 * |
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