CN103521084A - 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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- CN103521084A CN103521084A CN201310535586.7A CN201310535586A CN103521084A CN 103521084 A CN103521084 A CN 103521084A CN 201310535586 A CN201310535586 A CN 201310535586A CN 103521084 A CN103521084 A CN 103521084A
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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 sheet membrane, conventionally nonwoven supporting layer, ultrafiltration counterdie and separating layer, consists of.Separating layer Main Ingredients and Appearance is aromatic polyamides material, by interface polymerization reaction, forms, and 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.Conventionally have excellent hydrophilic reverse osmosis membrane and can make it to organic matter, microorganism and charged inorganic particulate, have very strong resistance tocrocking, 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 strengthening due to the active force producing by hydrogen bond or electrostatic attraction between film surface and hydrone.Therefore, the hydrophily of accurate evaluation counter-infiltration diaphragm is significant for improving its anti-pollution ability and water flux.
The contact angle that the hydrophily of reverse osmosis membrane utilizes liquid-autogenous cutting line and film-liquid interface to generate conventionally is at present evaluated, and test condition has a great impact the hydrophilic mensuration of reverse osmosis membrane.Hydrophilic impact is very important on reverse osmosis membrane for accurate hydrophily mensuration and complete understanding test condition, because this is conducive to improve the accuracy of testing result and the hydrophily of the different reverse osmosis membranes of accurate comparison; In addition, this also has great importance for analyzing the variation 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.Yet, although researcher understands the hydrophilic method of testing of reverse osmosis membrane so far, the impact of less concern test condition on testing result.Only have report seldom 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 the comparativity between certain reliability and scientific and different test results.
Summary of the invention
The technical problem to be solved in the present invention is to determine the hydrophilic test condition of contact angle method evaluation flat plate reverse osmosis film, be the impact of test condition on reverse osmosis membrane surface hydrophilicity, comprise sample pretreatment, ambient humidity, water temperature and salinity etc., the comprehensive flat plate reverse osmosis film of a kind of system hydrophily detection method is provided, sample pretreatment is simple, strong operability, has improved 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 film hydrophily method of testing, the method is carried out according to following steps:
(1) preprocessing process: get a counter-infiltration diaphragm, at room temperature counter-infiltration diaphragm is soaked through pure water, pure water rinsing, standby after vacuum drying;
(2) regulate and control test condition, envionmental humidity is 40%～70%, and probe temperature is 15～60 ℃, 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) tiling of pretreated counter-infiltration diaphragm is sticked on the sample stage of contact angle analyzer, 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 parameter to arrange, a droplet pure water or salt solution are dripped on counter-infiltration diaphragm, drop can obtain the static map of drop on counter-infiltration diaphragm after balance, utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating;
(5) in the operation of the diverse location repeating step (4) of counter-infiltration diaphragm repeatedly, then using repeatedly the mean value of test result as final contact angle result.
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 ℃, and be 20～24 hours drying time.
Preferably, the envionmental humidity in step (2) is 40%～60%.
Preferably, the probe temperature in step (2) is 15～40 ℃.
Preferably, the salinity range in step (2) is 0～6000mg/L.
Preferably, the number of operations of the repeating 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, the clear and definite preprocess method of flat plate reverse osmosis film hydrophily test process, proposition is controlled and is defined test conditions such as envionmental humidity, probe temperature and test fluid salinity, the comprehensive flat plate reverse osmosis film of the system of having set up 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 that final vacuum is dry, and cost is low, and process is simple, workable, is easy to promote.
(3) the present invention takes external factor impact into account in test process, Accurate Determining goes out the contact angle value on flat plate reverse osmosis film surface more, thereby judgement and the relatively hydrophily on reverse osmosis membrane surface, improved 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 sheet membrane, and detection method of the present invention proposes for this class flat plate reverse osmosis film just, and therefore, hydrophily detection technique of the present invention is practical, has important promotional value.
The specific embodiment
Below by specific embodiment, the present invention is further described in detail, 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 LP21 type low pressure reverse osmosis membrane component of producing from Guiyang Vontron Technology Co., Ltd. is taked the low pressure reverse osmosis diaphragm of 40mm * 5mm.At room temperature counter-infiltration diaphragm is immersed in 300ml pure water to 24 hours, then utilizes pure water rinsing 3 times, 60 ℃ of vacuum drying, after 24 hours, take out tiling and sticks 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 respectively 25 ℃ and 40%, probe temperature is 15 ℃, 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.
Adopt KUSS DSA100 contact angle analyzer (Germany) to carry out test analysis.To counter-infiltration diaphragm, wait drop on counter-infiltration diaphragm, after balance, can obtain the static map of drop one droplet test droplets.Utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating, during test, adopt static schema to carry out.In order to guarantee precision of analysis, at the diverse location of counter-infiltration diaphragm, detect 10 times, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycles 5000 μ s, burst lengths 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 LP21 type low pressure reverse osmosis membrane component of producing from Guiyang Vontron Technology Co., Ltd. is taked the low pressure reverse osmosis diaphragm of 40mm * 5mm.At room temperature counter-infiltration diaphragm is immersed in 300ml pure water to 18 hours, then utilizes pure water rinsing 4 times, 70 ℃ of vacuum drying, after 20 hours, take out tiling and sticks 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 respectively 25 ℃ and 50%, probe temperature is 25 ℃, 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.
Adopt KUSS DSA100 contact angle analyzer (Germany) to carry out test analysis.To counter-infiltration diaphragm, wait drop on counter-infiltration diaphragm, after balance, can obtain the static map of drop one droplet test droplets.Utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating, during test, adopt static schema to carry out.In order to guarantee precision of analysis, at the diverse location of counter-infiltration diaphragm, detect 8 times, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycles 5000 μ s, burst lengths 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 LP21 type low pressure reverse osmosis membrane component of producing from Guiyang Vontron Technology Co., Ltd. is taked the low pressure reverse osmosis diaphragm of 40mm * 5mm.At room temperature counter-infiltration diaphragm is immersed in 300ml pure water to 20 hours, then utilizes pure water rinsing 5 times, 65 ℃ of vacuum drying, after 22 hours, take out tiling and sticks 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 respectively 25 ℃ and 60%, probe temperature is 40 ℃, 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.
Adopt KUSS DSA100 contact angle analyzer (Germany) to carry out test analysis.To counter-infiltration diaphragm, wait drop on counter-infiltration diaphragm, after balance, can obtain the static map of drop one droplet test droplets.Utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating, during test, adopt static schema to carry out.In order to guarantee precision of analysis, at the diverse location of counter-infiltration diaphragm, detect 9 times, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycles 5000 μ s, burst lengths 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 LP21 type low pressure reverse osmosis membrane component of producing from Guiyang Vontron Technology Co., Ltd. is taked the low pressure reverse osmosis diaphragm of 40mm * 5mm.At room temperature counter-infiltration diaphragm is immersed in 300ml pure water to 24 hours, then utilizes pure water rinsing 3 times, 65 ℃ of vacuum drying, after 24 hours, take out tiling and sticks 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 respectively 25 ℃ and 70%, probe temperature is 60 ℃, 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.
Adopt KUSS DSA100 contact angle analyzer (Germany) to carry out test analysis.To counter-infiltration diaphragm, wait drop on counter-infiltration diaphragm, after balance, can obtain the static map of drop one droplet test droplets.Utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating, during test, adopt static schema to carry out.In order to guarantee precision of analysis, at the diverse location of counter-infiltration diaphragm, detect 9 times, then using mean value as final contact angle result.The parameter of instrument is set as respectively: voltage 60V, cycles 5000 μ s, burst lengths 100 μ s and a number are 100.
The contact angle of test gained low pressure reverse osmosis diaphragm is 40.2 °.
Counter-infiltration diaphragm is carried out after pretreatment, can be effectively except the protective agent of introducing in the superincumbent hydrophily fatty alcohol of some physical absorptions on striping surface and building-up process, reduce the impact of these materials on film surface hydrophilicity.Meanwhile, the test conditions such as test environment humidity, probe temperature, test fluid salinity carried out clear and definite and controlled, having strengthened the repeatability of result, having reduced the error of test, making between test result, to 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 above the preferred embodiments of the present invention are described; but the present invention is not limited to the above-mentioned specific embodiment; the above-mentioned specific embodiment is only schematic; be not restrictive; those of ordinary skill in the art is under enlightenment of the present invention; not departing from the scope situation that aim of the present invention and claim protect, can also make the concrete conversion of a lot of forms, within these all belong to 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 a counter-infiltration diaphragm, at room temperature counter-infiltration diaphragm is soaked through pure water, pure water rinsing, standby after vacuum drying;
(2) regulate and control test condition, envionmental humidity is 40%～70%, and probe temperature is 15～60 ℃, 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) tiling of pretreated counter-infiltration diaphragm is sticked on the sample stage of contact angle analyzer, 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 parameter to arrange, a droplet pure water or salt solution are dripped on counter-infiltration diaphragm, drop can obtain the static map of drop on counter-infiltration diaphragm after balance, utilize droplet profile analysis software the static map of drop to be analyzed and contact angle calculating;
(5) in the operation of the diverse location repeating step (4) of counter-infiltration diaphragm repeatedly, then using repeatedly the mean value of test result as final contact angle result.
2. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, it is characterized in that, the counter-infiltration diaphragm soak time in step (1) is 18～24 hours, and pure water rinsing number of times is 3～5 times, vacuum drying temperature is 60～70 ℃, and be 20～24 hours drying time.
3. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, 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, is characterized in that, the probe temperature in step (2) is 15～40 ℃.
5. a kind of flat plate reverse osmosis film hydrophily method of testing according to claim 1, 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, is characterized in that, the number of operations of the repeating step (4) in step (5) is 8～10 times.
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| CN107583467A (en) * | 2017-08-15 | 2018-01-16 | 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 |
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| 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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| CN107583467A (en) * | 2017-08-15 | 2018-01-16 | 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 |
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| 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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