CN103521084B - Method for testing hydrophilia of panel reverse osmosis membrane - Google Patents
Method for testing hydrophilia of panel reverse osmosis membrane Download PDFInfo
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- CN103521084B CN103521084B CN201310535586.7A CN201310535586A CN103521084B CN 103521084 B CN103521084 B CN 103521084B CN 201310535586 A CN201310535586 A CN 201310535586A CN 103521084 B CN103521084 B CN 103521084B
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Abstract
The invention discloses a method for testing the hydrophilia of a panel reverse osmosis membrane. According to the method, pretreatment comprises the steps of immersing the reverse osmosis membrane in pure water at the indoor temperature, washing the reverse osmosis membrane with the pure water, and carrying out vacuum drying on the reverse osmosis membrane to be prepared for use; regulating and controlling the relative humidity of the environment, test temperature and the salinity of a test solution; laying the membrane flat and sticking the membrane to a sample table of a contact angle analysis meter with a separation layer facing upwards and a supporting layer in contact with the sample table. The test is conducted with the static contact angle method, a small pure water or salt water drop is dripped onto the membrane after parameter setting of the contact angle analysis meter is regulated, a static diagram of the liquid drop can be obtained after the liquid drop is balanced on the membrane, and analysis and contact angle calculation are carried out on the static diagram of the liquid drop by means of liquid drop shape analysis software; the operation is repeated multiple times on different positions of the membrane, and an average value is obtained as the final contact angle result. According to the method for testing the hydrophilia of the panel reverse osmosis membrane, the pretreatment method of the testing process is defined, the concept that three testing conditions need to be controlled and defined is proposed, the reliability of the hydrophilia detecting method and the comparability of the detecting result are improved, and repeatability is high.
Description
Technical field
The present invention relates to the method for testing of reverse osmosis membrane separation layer surface characteristic, specifically, relate to the method for test slab reverse osmosis membrane surface hydrophilicity.
Background technology
Reverse osmosis membrane is widely used in fields such as seawater and brackish water desalination, bio-pharmaceuticals, chemical industry, purification of water qualitys.Current commercial reverse osmosis membrane mostly is aromatic polyamides Flat Membrane, is usually made up of non-woven fabrics supporting layer, ultrafiltration counterdie and separating layer.Separating layer Main Ingredients and Appearance is aromatic polyamides material, is formed by interface polymerization reaction, is the major function layer of reverse osmosis membrane.
The hydrophily of reverse osmosis membrane separation layer has material impact to its performance, particularly water flux and stain resistance.Usually having excellent hydrophilic reverse osmosis membrane can make it have very strong resistance tocrocking to organic matter, microorganism and charged inorganic particulate, this is because the stronger hydrophily in reverse osmosis membrane surface can weaken the interaction force between pollutant and film surface.In addition, the hydrophilic raising of reverse osmosis membrane can also improve its pure water flux, and this is the reason that the active force owing to being produced by hydrogen bond or electrostatic attraction between film surface and hydrone is strengthened.Therefore, accurate evaluation counter-infiltration diaphragm hydrophily for raising its anti-pollution ability and water flux significant.
The hydrophily of current reverse osmosis membrane utilizes liquid-autogenous cutting line and contact angle that film-liquid interface generates to evaluate usually, and test condition has a great impact the hydrophilic mensuration of reverse osmosis membrane.Accurate hydrophily measures and complete understanding test condition is very important on the hydrophilic impact of reverse osmosis membrane, because this is conducive to the hydrophily of the accuracy reverse osmosis membrane different from accurate comparison improving testing result; In addition, this also has great importance for analyzing the change with test condition of stain resistance and water flux.What is more important, research test condition contributes to film user optimization reverse osmosis membrane service condition to hydrophilic impact, improves its performance.But although researcher understands the hydrophilic method of testing of reverse osmosis membrane so far, less concern test condition is on the impact of testing result.Only have little report to relate to the correlation of reverse osmosis membrane hydrophily and test condition, and current also not about test condition to the hydrophilic sex system research of reverse osmosis membrane and report.This causes current reverse osmosis membrane hydrophilicity method of testing to lack comparativity between certain reliability and scientific and different test result.
Summary of the invention
The technical problem to be solved in the present invention determines that contact angle method evaluates the hydrophilic test condition of flat plate reverse osmosis film, namely test condition is on the impact of reverse osmosis membrane surface hydrophilicity, comprise sample pretreatment, ambient humidity, water temperature and salinity etc., a kind of system comprehensive flat plate reverse osmosis film hydrophily detection method is provided, sample pretreatment is simple, strong operability, improves the reliability of hydrophily detection method and the comparativity of testing result.
In order to solve the problems of the technologies described above, the present invention is achieved by following technical scheme:
A kind of flat plate reverse osmosis film hydrophily method of testing, the method is carried out according to following steps:
(1) preprocessing process: get one piece of counter-infiltration diaphragm, at room temperature counter-infiltration diaphragm is soaked through pure water, pure water rinsing, for subsequent use after vacuum drying;
(2) regulate and control test condition, envionmental humidity is 40% ~ 70%, and probe temperature is 15 ~ 60 DEG C, and the salinity of test fluid is 0 ~ 10000mg/L; Test fluid temperature is all consistent with probe temperature with diaphragm temperature, and the salinity of test fluid represents with sodium chloride content in test fluid;
(3) be pasted onto on the sample stage of contact angle analyzer by the tiling of pretreated counter-infiltration diaphragm, separating layer upwards and supporting layer contacts with sample stage;
(4) test adopts Static Contact horn cupping to carry out, after regulating contact angle analyzer optimum configurations, a droplet pure water or salt solution are dripped on counter-infiltration diaphragm, drop can obtain the static map of drop after balancing on counter-infiltration diaphragm, utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating;
(5) operation of step (4) is repeated repeatedly, then using the mean value of repeatedly test result as final contact angle result at the diverse location of counter-infiltration diaphragm.
Preferably, the counter-infiltration diaphragm soak time in step (1) is 18 ~ 24 hours, and pure water rinsing number of times is 3 ~ 5 times, and vacuum drying temperature is 60 ~ 70 DEG C, and drying time is 20 ~ 24 hours.
Preferably, the envionmental humidity in step (2) is 40% ~ 60%.
Preferably, the probe temperature in step (2) is 15 ~ 40 DEG C.
Preferably, the salinity range in step (2) is 0 ~ 6000mg/L.
Preferably, the number of operations of the repetition step (4) in step (5) is 8 ~ 10 times.
The invention has the beneficial effects as follows:
(1) the present invention is in conjunction with the practical operation situation of reverse osmosis membrane, specify that the preprocess method of flat plate reverse osmosis film hydrophily test process, propose to control test conditions such as envionmental humidity, probe temperature and test fluid salinity and define, the system that establishes comprehensive flat plate reverse osmosis film hydrophily method of testing, fills up test condition to the hydrophilic sex blank of flat plate reverse osmosis film.
(2) sample pretreatment process of the present invention adopts first pure water to soak, the step of final vacuum drying, and cost is low, and process is simple, workable, is easy to promote.
(3) external factor impact is taken into account by the present invention in test process, more can go out the contact angle values on flat plate reverse osmosis film surface by Accurate Determining, thus judge and compare the hydrophily on reverse osmosis membrane surface, improve the reliability of hydrophily detection method and the comparativity of testing result, repeatable strong.
(4) current commercial reverse osmosis membrane mostly is aromatic polyamides Flat Membrane, and detection method of the present invention proposes for this kind of flat plate reverse osmosis film just, and therefore, hydrophily detection technique of the present invention is practical, has important promotional value.
Detailed description of the invention
Be further described in detail the present invention below by specific embodiment, the flat plate reverse osmosis film in following examples is commercialization counter-infiltration diaphragm, is specially the LP21 type low-pressure reverse osmosis membrane that Guiyang Vontron Technology Co., Ltd. produces.
Embodiment 1
The low pressure reverse osmosis diaphragm of 40mm × 5mm is taked from the LP21 type low pressure reverse osmosis membrane component of Guiyang Vontron Technology Co., Ltd.'s production.At room temperature counter-infiltration diaphragm to be immersed in 300ml pure water 24 hours, then to utilize pure water rinsing 3 times, 60 DEG C of vacuum drying after 24 hours, take out tiling and be pasted onto on sample stage, separating layer upward.
Regulate test environment conditions, during test, use constant temperature and humidity system set environment temperature and relative humidity to be set as 25 DEG C and 40% respectively, probe temperature is 15 DEG C, use baking oven or refrigerator that the temperature of counter-infiltration diaphragm and test fluid is adjusted to probe temperature, the salinity of test fluid is 0mg/L.
KUSS DSA100 contact angle analyzer (Germany) is adopted to carry out test analysis.By a droplet test droplets on counter-infiltration diaphragm, the static map of drop after waiting drop to balance on counter-infiltration diaphragm, can be obtained.Utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating, during test, adopt static schema to carry out.In order to ensure precision of analysis, detect 10 times at the diverse location of counter-infiltration diaphragm, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycle 5000 μ s, burst length 100 μ s and a number are 100.
The contact angle of test gained low pressure reverse osmosis diaphragm is 57.3 °.
Embodiment 2
The low pressure reverse osmosis diaphragm of 40mm × 5mm is taked from the LP21 type low pressure reverse osmosis membrane component of Guiyang Vontron Technology Co., Ltd.'s production.At room temperature counter-infiltration diaphragm to be immersed in 300ml pure water 18 hours, then to utilize pure water rinsing 4 times, 70 DEG C of vacuum drying after 20 hours, take out tiling and be pasted onto on sample stage, separating layer upward.
Regulate test environment conditions, during test, use constant temperature and humidity system environment temperature and relative humidity to be set as 25 DEG C and 50% respectively, probe temperature is 25 DEG C, use baking oven that the temperature of counter-infiltration diaphragm and test fluid is adjusted to probe temperature, the salinity of test fluid is 2000mg/L.
KUSS DSA100 contact angle analyzer (Germany) is adopted to carry out test analysis.By a droplet test droplets on counter-infiltration diaphragm, the static map of drop after waiting drop to balance on counter-infiltration diaphragm, can be obtained.Utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating, during test, adopt static schema to carry out.In order to ensure precision of analysis, detect 8 times at the diverse location of counter-infiltration diaphragm, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycle 5000 μ s, burst length 100 μ s and a number are 100.
The contact angle of test gained low pressure reverse osmosis diaphragm is 48.6 °.
Embodiment 3
The low pressure reverse osmosis diaphragm of 40mm × 5mm is taked from the LP21 type low pressure reverse osmosis membrane component of Guiyang Vontron Technology Co., Ltd.'s production.At room temperature counter-infiltration diaphragm to be immersed in 300ml pure water 20 hours, then to utilize pure water rinsing 5 times, 65 DEG C of vacuum drying after 22 hours, take out tiling and be pasted onto on sample stage, separating layer upward.
Regulate test environment conditions, during test, use constant temperature and humidity system environment temperature and relative humidity to be set as 25 DEG C and 60% respectively, probe temperature is 40 DEG C, use baking oven that the temperature of counter-infiltration diaphragm and test fluid is adjusted to probe temperature, the salinity of test fluid is 6000mg/L.
KUSS DSA100 contact angle analyzer (Germany) is adopted to carry out test analysis.By a droplet test droplets on counter-infiltration diaphragm, the static map of drop after waiting drop to balance on counter-infiltration diaphragm, can be obtained.Utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating, during test, adopt static schema to carry out.In order to ensure precision of analysis, detect 9 times at the diverse location of counter-infiltration diaphragm, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycle 5000 μ s, burst length 100 μ s and a number are 100.
The contact angle of test gained low pressure reverse osmosis diaphragm is 44.7 °.
Embodiment 4
The low pressure reverse osmosis diaphragm of 40mm × 5mm is taked from the LP21 type low pressure reverse osmosis membrane component of Guiyang Vontron Technology Co., Ltd.'s production.At room temperature counter-infiltration diaphragm to be immersed in 300ml pure water 24 hours, then to utilize pure water rinsing 3 times, 65 DEG C of vacuum drying after 24 hours, take out tiling and be pasted onto on sample stage, separating layer upward.
Regulate test environment conditions, during test, use constant temperature and humidity system environment temperature and relative humidity to be set as 25 DEG C and 70% respectively, probe temperature is 60 DEG C, use baking oven that the temperature of counter-infiltration diaphragm and test fluid is adjusted to probe temperature, the salinity of test fluid is 10000mg/L.
KUSS DSA100 contact angle analyzer (Germany) is adopted to carry out test analysis.By a droplet test droplets on counter-infiltration diaphragm, the static map of drop after waiting drop to balance on counter-infiltration diaphragm, can be obtained.Utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating, during test, adopt static schema to carry out.In order to ensure precision of analysis, detect 9 times at the diverse location of counter-infiltration diaphragm, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycle 5000 μ s, burst length 100 μ s and a number are 100.
The contact angle of test gained low pressure reverse osmosis diaphragm is 40.2 °.
After pretreatment is carried out to counter-infiltration diaphragm, effectively except the protective agent introduced in the superincumbent hydrophily fatty alcohol of some physical absorptions on striping surface and building-up process, the impact of these materials on film surface hydrophilicity can be reduced.Meanwhile, the test conditions such as test environment humidity, probe temperature, test fluid salinity carried out clear and definite and control, enhancing the repeatability of result, decrease the error of test, make, between test result, there is comparativity.Propose to use sodium-chloride water solution as test fluid, closer to the actual motion environment of counter-infiltration diaphragm, test result has more practical significance.
Although be described the preferred embodiments of the present invention above; but the present invention is not limited to above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; do not departing under the ambit that present inventive concept and claim protect, can also make the concrete conversion of a lot of form, these all belong within protection scope of the present invention.
Claims (6)
1. a flat plate reverse osmosis film hydrophily method of testing, is characterized in that, the method is carried out according to following steps:
(1) preprocessing process: get one piece of counter-infiltration diaphragm, at room temperature counter-infiltration diaphragm is soaked through pure water, pure water rinsing, for subsequent use after vacuum drying;
(2) regulate and control test condition, envionmental humidity is 40% ~ 70%, and probe temperature is 15 ~ 60 DEG C, and the salinity of test fluid is 0 ~ 10000mg/L; Test fluid temperature is all consistent with probe temperature with diaphragm temperature, and the salinity of test fluid represents with sodium chloride content in test fluid;
(3) be pasted onto on the sample stage of contact angle analyzer by the tiling of pretreated counter-infiltration diaphragm, separating layer upwards and supporting layer contacts with sample stage;
(4) test adopts Static Contact horn cupping to carry out, after regulating contact angle analyzer optimum configurations, a droplet pure water or salt solution are dripped on counter-infiltration diaphragm, drop can obtain the static map of drop after balancing on counter-infiltration diaphragm, utilize the static map of Drop Shape Analysis software to drop to analyze and contact angle calculating;
(5) operation of step (4) is repeated repeatedly, then using the mean value of repeatedly test result as final contact angle result at the diverse location of counter-infiltration diaphragm;
Described counter-infiltration diaphragm is aromatic polyamides Flat Membrane.
2. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, counter-infiltration diaphragm soak time in step (1) is 18 ~ 24 hours, pure water rinsing number of times is 3 ~ 5 times, vacuum drying temperature is 60 ~ 70 DEG C, and drying time is 20 ~ 24 hours.
3. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, the envionmental humidity in step (2) is 40% ~ 60%.
4. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, the probe temperature in step (2) is 15 ~ 40 DEG C.
5. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, the salinity range in step (2) is 0 ~ 6000mg/L.
6. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, the number of operations of the repetition step (4) in step (5) is 8 ~ 10 times.
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| CN107583467B (en) * | 2017-08-15 | 2019-10-22 | 深圳安吉尔饮水产业集团有限公司 | A kind of method and device for testing reverse osmosis membrane |
| CN109752389A (en) * | 2017-11-07 | 2019-05-14 | 隆基绿能科技股份有限公司 | sheet surface cleanliness measurement method |
| CN108927011A (en) * | 2018-07-27 | 2018-12-04 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of rolling sea-water reverse osmose membrane component boron-removing rate test method |
| CN108926998A (en) * | 2018-07-27 | 2018-12-04 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of rolling bitter reverse-osmosis membrane element boron-removing rate test method |
| CN108970413A (en) * | 2018-07-27 | 2018-12-11 | 国家海洋局天津海水淡化与综合利用研究所 | A kind of plate bitter reverse osmosis membrane boron-removing rate test method |
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| CN101033951A (en) * | 2007-02-02 | 2007-09-12 | 福耀集团双辽有限公司 | Online measuring method of self clean glass contact angle |
| CN102167280A (en) * | 2011-01-13 | 2011-08-31 | 西北工业大学 | Super-hydrophobic silicon micron-nano composite structure and preparation method thereof |
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