CN112808015A - Detection method and device for hollow fiber membrane - Google Patents
Detection method and device for hollow fiber membrane Download PDFInfo
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- CN112808015A CN112808015A CN202011559018.7A CN202011559018A CN112808015A CN 112808015 A CN112808015 A CN 112808015A CN 202011559018 A CN202011559018 A CN 202011559018A CN 112808015 A CN112808015 A CN 112808015A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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
- G01D—MEASURING NOT SPECIALLY ADAPTED FOR A SPECIFIC VARIABLE; ARRANGEMENTS FOR MEASURING TWO OR MORE VARIABLES NOT COVERED IN A SINGLE OTHER SUBCLASS; TARIFF METERING APPARATUS; MEASURING OR TESTING NOT OTHERWISE PROVIDED FOR
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Abstract
A detection method of a hollow fiber membrane comprises the following steps: measuring a certain length of the hollow fiber membrane yarn, and fastening two ends of the hollow fiber membrane yarn by using ropes to obtain a membrane yarn assembly; and measuring the parameters of retention rate, pure water flux and bubble point pressure of the membrane wire assembly. The detection method is simple to operate, saves cost, reduces energy consumption, is quick, can timely respond problems to research and production personnel, timely adjusts production, and avoids waste of raw materials.
Description
Technical Field
The invention relates to the technical field of detection, in particular to a detection device and a detection method for a hollow fiber membrane.
Background
Currently, with the rapid development of global economy and the growth of global population, water resource problems are increasing, for example: water shortage, water quality pollution and waste caused by insufficient utilization of water resources. Finding a safe and efficient solution is now an important issue in development today. Membrane separation techniques exhibit a number of advantages in solving the water treatment problem: low energy consumption, environmental protection, high separation efficiency and the like. The hollow fiber membrane is one of the membrane varieties which are developed rapidly internationally in recent years, and the existing hollow fiber membrane materials are many and have different forms.
The PVDF hollow fiber external pressure film is put into production on line, and the PVDF hollow fiber external pressure film is required to be checked according to corresponding standards so as to judge whether the produced film yarn meets the use requirement or not, and the film yarn meeting the requirement can be used for manufacturing a component and is put into use. However, the existing detection method is complex, high in energy consumption and complex in device structure, and can not rapidly detect whether the membrane filaments are qualified or not.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide a detection method of a hollow fiber membrane, which is characterized in that a membrane wire assembly obtained by cutting a small part of hollow fiber membrane wires is used for carrying out interception, pure water flux and bubble point pressure tests on the membrane wire assembly, so that the cost is saved, the energy consumption is reduced, the test method is rapid, problems can be timely reflected to research and production personnel, the production can be timely adjusted, and the waste of raw materials is avoided.
The second purpose of the invention is to provide a detection device for hollow fiber membranes, which can determine the quality of the whole batch of hollow fiber membrane filaments by measuring the membrane filament assembly, has a simple structure, can quickly obtain a test result and react to research and production personnel, and can timely adjust production to avoid waste of raw materials.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a detection method of a hollow fiber membrane, which comprises the following steps:
measuring a certain length of the hollow fiber membrane yarn, and fastening two ends of the hollow fiber membrane yarn by using ropes to obtain a membrane yarn assembly;
and measuring the parameters of retention rate, pure water flux and bubble point pressure of the membrane wire assembly.
In the prior art, in order to measure the data of the interception rate, the pure water flux and the bubble point pressure of the hollow fiber membrane filaments, a plurality of hollow fiber membrane filaments are often intercepted, unnecessary waste is caused, the test method is complicated, the obtained result is slow, and the waste of raw materials is caused because the hollow fiber membrane filaments cannot react in time to research and production personnel.
In order to solve the technical problems, the invention provides a detection method of a hollow fiber membrane, which is characterized in that a small part of a hollow fiber membrane wire is cut to obtain a membrane wire assembly, the membrane wire assembly is inserted into a detection device, and pure water flux, rejection rate and bubble point pressure are respectively tested. The cost is saved by arranging the membrane wire assembly, the testing method is simplified, the time for obtaining results is shortened, and the adjustment of research and production personnel is facilitated.
Preferably, the method for measuring the retention rate comprises: the concentration of a raw material solution is measured firstly to obtain C1, then the concentration of a discharged material solution passing through the membrane wire assembly is measured to obtain C2, and finally the concentration is calculated by using a formula Ru ═ C1-C2)/C1 multiplied by 100%, wherein the unit of C1 and C2 is mg/L. The raw material liquid for measuring the rejection rate is polyoxyethylene, a small amount of the raw material polyoxyethylene in the raw material tank is taken out firstly and placed in a beaker, and the concentration is measured. And starting a detection device, allowing the raw material polyoxyethylene to enter the measuring cylinder after passing through the membrane wire assembly, taking a small amount of discharged polyoxyethylene in the measuring cylinder, placing the discharged polyoxyethylene in a beaker, and measuring the concentration. The method for measuring the concentration of the raw material polyoxyethylene and the discharged polyoxyethylene is absorbance test, an ultraviolet visible spectrophotometer is preheated for 20min, and the raw material polyoxyethylene and the discharged polyoxyethylene for detection are configured: adding a bismuth potassium iodide reagent and an acetic acid-sodium acetate buffer solution into the prepared raw material polyoxyethylene beaker and the discharged polyoxyethylene beaker, adding distilled water for dilution, shaking up and fixing the volume. And (3) timing and placing for 12min after constant volume, measuring absorbance on an ultraviolet visible spectrophotometer by using a 1cm cuvette under the wavelength of 510nm, and recording test data into an electronic document to calculate the concentrations of the raw material polyoxyethylene and the discharged polyoxyethylene.
Preferably, the method for measuring the pure water flux comprises: q, t of the membrane-filament assembly was measured, and after the measurement, the pure water flux F was calculated using the following formula:
a ═ n pi DL, where:
a- - - -membrane area in m2；
n is the number of the hollow fiber membranes;
d is the diameter of the hollow fiber membrane, and the unit is m;
l- - -the effective length of the hollow fiber membrane, in m;
then calculating the pure water flux according to the membrane area
In the formula:
f- -pure water flux in L/(m)2.h)；
Q- - -pure water permeability, unit is L;
a- - - -membrane area in m2；
t- -the time taken to collect the pure water permeation in units of h.
When the membrane area A is measured, the number n of the hollow fiber membranes can be simply counted, the diameter D of the hollow fiber membranes is measured by using a reading microscope, the effective length L of the hollow fiber membranes is obtained by using a ruler, and the membrane area A can be calculated by the data. The raw material liquid when measuring pure water flux is the pure water, starts detection device, control governing valve, and when the reading of manometer reached 0.1Mpa, the pure water of following the separation of membrane silk subassembly was taken in the grafting with the graduated flask, and timing 1 minute reads the volume of pure water in the graduated flask promptly and is pure water permeability Q, calculates pure water flux according to the formula.
Preferably, the Q, t of the membrane-yarn assembly is measured by a method comprising: and measuring the amount Q of water flowing through the membrane wire assembly within a certain time t, wherein the time t for collecting the pure water permeation amount is a specific time, and the amount of pure water collected within the time for collecting the pure water permeation amount is the pure water permeation amount. The measurement time t is 1 minute, so that accurate data can be obtained in a short time. The measurement time t is 1 minute because time is wasted due to long time and inaccurate data due to short time. In this 1 minute period, the volume of the pure water taken in with the measuring cylinder was defined as the pure water permeation amount Q.
The invention also provides a detection device of the hollow fiber membrane, which comprises a membrane wire component, a raw material tank, a measuring cylinder, a tension tester and a bubble point tester, wherein the membrane wire component is arranged between the raw material tank and the measuring cylinder to realize the determination of the retention rate and the pure water flux, and the bubble point tester is in non-contact connection to realize the detection of the tensile property and the bubble point pressure of the membrane wire component. When the detection device detects the retention rate and the pure water flux, the membrane wire assembly is inserted into the detection device to form a closed loop. When the membrane wire assembly detects the bubble point pressure, the membrane wire assembly is taken out of the detection device and placed on a bubble point pressure tester to measure the bubble point pressure.
Preferably, a regulating valve is arranged between the raw material tank and the membrane wire assembly, and the quantity of liquid flowing through the membrane wire assembly is regulated by the control of the regulating valve.
Preferably, a water suction pump for providing motion power for the liquid in the raw material tank is arranged between the raw material tank and the membrane wire assembly.
Preferably, a pressure gauge is included between the regulating valve and the membrane wire assembly to realize the liquid communication under certain pressure conditions.
Above-mentioned head tank, the graduated flask, the membrane silk subassembly, the suction pump, through the pipe connection between governing valve and the manometer, open the suction pump and provide power for liquid circulates in the pipeline, the governing valve can be adjusted the liquid volume of membrane silk subassembly of flowing through in the pipeline, the governing valve has also adjusted the pressure in the pipeline simultaneously when adjusting the pipeline internal liquid flow, according to the reading control governing valve on the manometer, just so can realize measuring the membrane silk subassembly under certain pressure condition.
The detection device can measure the quality of the whole batch of hollow fiber membrane yarns by measuring the membrane yarn assembly, has a simple structure, can quickly obtain a test result and react to research and production personnel, regulates production in time and avoids waste of raw materials.
Compared with the prior art, the invention has the beneficial effects that:
(1) according to the hollow fiber membrane detection method, the membrane wire assembly obtained by cutting a small part of the hollow fiber membrane wires is used for intercepting the membrane wire assembly and testing the pure water flux and the bubble point pressure, so that the cost is saved, the energy consumption is reduced, the test method is rapid, the problems can be timely reflected to research and production personnel, the production can be timely adjusted, and the waste of raw materials is avoided.
(2) The hollow fiber membrane detection device provided by the invention can be used for measuring the quality of the whole batch of hollow fiber membrane filaments by measuring the membrane filament assembly, has a simple structure and less material consumption, can be used for quickly obtaining a test result and reacting the test result to research and production personnel, and avoids the waste of raw materials.
Drawings
Various other advantages and benefits will become apparent to those of ordinary skill in the art upon reading the following detailed description of the preferred embodiments. The drawings are only for purposes of illustrating the preferred embodiments and are not to be construed as limiting the invention. Also, like reference numerals are used to refer to like parts throughout the drawings. In the drawings:
fig. 1 is a schematic structural diagram of a detection apparatus for a hollow fiber membrane according to an embodiment of the present invention.
Wherein:
10-a raw material tank; 20-adjusting the valve;
30-pressure gauge; 40-membrane thread component;
50-water pump; and 60-measuring cylinder.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. 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.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
In order to more clearly illustrate the technical solution of the present invention, the following description is made in the form of specific embodiments.
Examples
Referring to fig. 1, the present embodiment provides a detection apparatus for a hollow fiber membrane, including a membrane wire assembly 40, a raw material tank 10, a measuring cylinder 60, an adjusting valve 20, a pressure gauge 30, a water pump 50, and a bubble point tester, where the membrane wire assembly 40 is disposed between the raw material tank 10 and the measuring cylinder 60 to measure the rejection rate and the pure water flux, and the bubble point tester is connected in a non-contact manner to detect the bubble point pressure of the membrane wire assembly 40. The regulating valve 20 is arranged between the raw material tank 10 and the membrane wire assembly 40, and the regulating valve 20 is controlled to regulate the amount of liquid flowing through the membrane wire assembly 40. A suction pump 50 is provided between the raw material tank 10 and the membrane wire assembly 40 to power the liquid in the sensing device, and a pressure gauge 30 is provided between the regulating valve 20 and the membrane wire assembly 40 to read the pressure in the sensing device. According to the flowing direction of the liquid, the rear side of a raw material tank 10 is connected with an adjusting valve 20, the rear side of the adjusting valve 20 is connected with a pressure gauge 30, the rear side of the pressure gauge 30 is connected with a membrane wire assembly 40, the rear side of the membrane wire assembly 40 is connected with a water pump 50, the liquid of the water pump 50 returns to the raw material tank 10, and a measuring cylinder 60 is arranged below the membrane wire assembly 30 to take the intercepted liquid.
The detection method for obtaining the hollow fiber membrane by the detection device is connected according to the detection device and comprises the following steps: firstly, a small section of hollow fiber membrane wire is taken down from a hollow fiber membrane wire winding wheel, and the section of hollow fiber membrane wire is put into a constant temperature water bath kettle to be washed and removed with impurities. Then one end of the hollow fiber membrane wire is inserted into a needle head and tightly bound by a rope, the other end of the hollow fiber membrane wire is tightly bound by the rope after being folded, the redundant part leaked outside the rope is reduced to obtain a membrane wire assembly 40, the membrane wire assembly 40 is subjected to advanced measurement, firstly, the membrane wire assembly 40 is counted to be composed of several hollow fiber membranes to obtain the number n of the hollow fiber membranes, then, one hollow fiber membrane is taken out and measured by an electronic reading microscope to obtain the diameter D of the hollow fiber membrane, finally, the effective length L of the hollow fiber membrane is measured by a ruler, and the membrane area A is calculated according to the membrane area A which is n pi DL.
Secondly, performing a pure water flux test on the membrane wires, adding pure water into the raw material tank 10, heating to 25 ℃, and using at a constant temperature; the membrane-wire assembly 40 prepared above is inserted into the test device, the suction pump 50 is turned on to power the flow of pure water, then the regulating valve 20 is opened, the reading of the pressure gauge 30 is observed, and the pressure inside the test device is adjusted by controlling the regulating valve 20. When the regulating valve 20 is controlled, when the pointer of the pressure gauge 30 is 0.1Mpa, the measuring cylinder 60 is used for receiving the water dripped from the membrane wire assembly 30, the time is kept for 1 minute, the volume of the liquid in the measuring cylinder is recorded to obtain the pure water permeation quantity Q, and the pure water permeation quantity Q is obtained according to the pure water flux quantity
Pure water flux F is calculated.
The membrane wire assembly 40 is then tested for rejection. Firstly, acetic acid-sodium acetate buffer solution, bismuth potassium iodide solution and polyethylene oxide solution to be used are prepared. The preparation steps of the acetic acid-sodium acetate buffer solution are as follows:
(1) 16.406g of sodium acetate were weighed out accurately and placed in a 100mL beaker, and the appropriate amount of water was added and allowed to dissolve. Transferring the solution into a 100mL volumetric flask, adding water to the scale mark, shaking up, and preparing into 0.2mol/L sodium acetate solution;
(2) 6.005g of glacial acetic acid was weighed accurately and placed in a 50mL beaker, and the appropriate amount of water was added and allowed to dissolve. Transferring the solution into a 500mL volumetric flask, adding water to the scale mark, and shaking to prepare a 0.2mol/L glacial acetic acid solution;
(3) 590mL of 0.2mol/L sodium acetate solution and 410mL of 0.2mol/L glacial acetic acid solution are measured and placed in a 1000mL volumetric flask to prepare acetic acid-sodium acetate buffer solution with pH4.8.
The preparation method of the potassium bismuth iodide solution comprises the following steps:
(1) 0.800g of bismuth subnitrate was accurately weighed and placed in a 50mL beaker, and 10.0mL of anhydrous acetic acid and an appropriate amount of water were added to dissolve it. Transferring the solution into a 50mL volumetric flask, adding water to the scale mark, and shaking up;
(2) accurately weighing 20.000g of potassium iodide, placing the potassium iodide in a 50mL beaker, adding a proper amount of water to dissolve the potassium iodide, transferring the solution to a 50mL brown volumetric flask, adding water to a scale mark, and shaking up;
(3) respectively transferring 5.0mL of the solution prepared in the step (1) and 5mL of the solution prepared in the step (2) into a 100mL brown volumetric flask, adding 40.0mL of anhydrous acetic acid, adding water to a scale mark, shaking up, and preparing the bismuth potassium iodide solution.
The polyethylene oxide solution is prepared by the following steps:
selecting polyoxyethylene with a molecular weight of 100000, accurately weighing 20g of polyoxyethylene, dissolving the polyoxyethylene in two 500mL beakers, carrying out ultrasonic reaction until no agglomeration exists in the solution, stirring the polyoxyethylene for multiple times by using a glass rod during the ultrasonic reaction, then moving the polyoxyethylene into a 5L plastic measuring cup, flushing the two 500mL beakers, pouring liquid into the 5L plastic measuring cup, adding water to a constant volume of 4L, and stirring the polyoxyethylene by using the glass rod to ensure that the solution is uniformly distributed to prepare a 5000mg/L polyoxyethylene solution.
After obtaining acetic acid-sodium acetate buffer solution, bismuth potassium iodide solution and polyethylene oxide solution, the retention rate test is carried out, and the steps are as follows:
(1) before the interception test operation, a small amount of polyoxyethylene solution is taken out and placed in a small beaker for standby;
(2) 4L of polyoxyethylene solution is poured into the raw material tank 10, the power supply is switched on, the water pump 50 is started, and the residual solution in the detection device is replaced and washed. The prepared membrane wire assembly 40 is connected to a detection device in a quick-plug mode, a polyethylene oxide solution passes through the membrane wire assembly 40, the operation is carried out for about 5min, and a 50mL beaker with a sequence number is used for receiving in a measuring cylinder 60 for about 2 h. Transferring the small amount of the polyoxyethylene solution prepared in the step (1) into a volumetric flask with the label a for standby by using a liquid transfer gun or a pipette, and then transferring 25mL of trapped fluid into a volumetric flask with the label b for standby by using the liquid transfer gun or the pipette;
(3) and (5) testing the absorbance. Preheating an ultraviolet-visible spectrophotometer for 20min, and preparing a solution for detection: and (3) adding 5mL of bismuth potassium iodide reagent and 5mL of acetic acid-sodium acetate buffer solution into the 50mL volumetric flask a and the volumetric flask b prepared in the step (2), respectively adding distilled water to dilute to a scale, shaking up and fixing the volume. After the volumetric flask a is subjected to constant volume, the volumetric flask a is placed for 12min in a timing mode, a 1cm cuvette is used for measuring the absorbance on an ultraviolet-visible spectrophotometer under the wavelength of 510nm, the volumetric flask b is operated by the same method, the test data of the volumetric flask a and the volumetric flask b are recorded into an electronic document, and the retention rates C1 and C2 are calculated, wherein C1 is the concentration of the volumetric flask a, and C2 is the concentration of the volumetric flask b, and the unit is mg/L.
(4) Calculating the retention rate Ru ═ C1-C2)/C1×100％。
Finally, take off membrane silk subassembly 40, with membrane silk subassembly 40 with insert the form soon and connect to bubble point pressure tester on, test membrane silk bubble point pressure and record data.
In a word, the detection method of the hollow fiber membrane is simple to operate, saves cost, reduces energy consumption, is quick in test method, can timely respond problems to research and production personnel, timely adjusts production, and avoids waste of raw materials.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. A detection method of a hollow fiber membrane is characterized by comprising the following steps:
measuring a certain length of the hollow fiber membrane yarn, and fastening two ends of the hollow fiber membrane yarn by using ropes to obtain a membrane yarn assembly;
and measuring the parameters of retention rate, pure water flux and bubble point pressure of the membrane wire assembly.
2. The detection method according to claim 1, wherein the determination method of the retention rate comprises: first, the concentration C of the raw material liquid is measured1Then testing the concentration C of discharged liquid passing through the membrane yarn assembly2Finally, the formula Ru ═ C (C) is used1-C2)/C1X 100% is calculated as1、C2The unit of (b) is mg/L.
3. The method for detecting according to claim 1, wherein the method for measuring pure water flux comprises: q, t of the membrane-filament assembly was measured, and after the measurement, the pure water flux F was calculated using the following formula:
a ═ n pi DL, where:
a- - - -membrane area in m2；
n is the number of the hollow fiber membranes;
d is the diameter of the hollow fiber membrane, and the unit is m;
l- - -the effective length of the hollow fiber membrane, in m;
then calculating the pure water flux according to the membrane area
In the formula:
f- -pure water flux in L/(m)2.h)；
Q- - -pure water permeability, unit is L;
a- - - -membrane area in m2；
t- -the time taken to collect the pure water permeation in units of h.
4. The method of detecting according to claim 3, wherein the step of measuring Q, t for the membrane-wire assembly comprises: and measuring the amount Q of water flowing through the membrane wire assembly within a certain time t, wherein the time t for collecting the pure water permeation amount is a specific time, and the amount of pure water collected within the time for collecting the pure water permeation amount is the pure water permeation amount.
5. A hollow fiber membrane test device used in the test method according to any one of claims 1 to 4, comprising a membrane wire module, a stock tank, a measuring cylinder, and a bubble point tester, wherein the membrane wire module is disposed between the stock tank and the measuring cylinder to measure the retention rate and the pure water flux, and the bubble point tester is connected in a non-contact manner to measure the tensile property and the bubble point pressure of the membrane wire module.
6. The detection device according to claim 5, wherein a regulating valve is arranged between the raw material tank and the membrane-wire assembly, and the regulating valve is used for controlling to regulate the amount of liquid flowing through the membrane-wire assembly.
7. The detection apparatus according to claim 5, wherein a suction pump is provided between the raw material tank and the membrane wire assembly for providing a motive power to the liquid in the raw material tank.
8. The testing device of claim 6, wherein a pressure gauge is included between the regulating valve and the membrane wire assembly to allow fluid communication under certain pressure conditions.
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