This standard specifies the test methods for tubular (including single tube and multi-channel) ceramic microporous filter membranes: the test methods for maximum pore size and pure water flux, average pore size, porosity, bending strength and acid and alkali corrosion resistance, and is applicable to the testing of tubular ceramic microporous filter membranes. HY/T 064-2002 Test methods for tubular ceramic microporous filter membranes HY/T064-2002 standard download decompression password: www.bzxz.net
This standard specifies the test methods for tubular (including single tube and multi-channel) ceramic microporous filter membranes: the test methods for maximum pore size and pure water flux, average pore size, porosity, bending strength and acid and alkali corrosion resistance, and is applicable to the testing of tubular ceramic microporous filter membranes.

ICS07.060;67.260
Marine Industry Standard of the People's Republic of China
HY/T064—2002
Test methods for tubular ceramic microporous filtration membrane2002-12-30 Issued
State Oceanic Administration Issued
2003-02-01 Implementation
Nichisheng Standard Nanny
HY/T064-—2002
Appendix A of this standard is the appendix of the standard.
Appendix B of this standard is the appendix of the suggestion.
This standard is proposed by China Membrane Industry Association. This standard is under the jurisdiction of the National Marine Standard and Metrology Center. Foreword
This standard was drafted by: Membrane Science and Technology Institute of Nanjing University of Technology, Jiangsu Jiuwu High-tech Co., Ltd. The main drafters of this standard are Xing Weihong, Huang Pei, Fan Yiqun, Wang Huailin, Bai Wenjing and Jing Wenheng. Marine Industry Standard of the People's Republic of China
Test methods for tubular ceramic microporous filtration membrane
Test methods for tubular ceramic microporous filtration membrane1Scope
HY/T 064-2002
This standard specifies the test methods for tubular (including single-tube and multi-channel) ceramic microporous filtration membranes: test methods for maximum pore size and pure water flux, average pore size, porosity, bending strength and acid and alkali corrosion resistance. This standard is applicable to the testing of tubular ceramic microporous filtration membrane elements. 2 Referenced standards
The provisions contained in the following standards constitute the provisions of this standard by reference in this standard. When this standard is published, the versions shown are valid. All standards are subject to revision, and parties using this standard should explore the possibility of using the latest versions of the following standards. GB/T1966—1996 Test method for apparent porosity and bulk density of porous ceramics GB17323---1998 Bottled drinking pure water 3 Definitions
This standard adopts the following definitions.
3.1 Dry membrane
Dry membrane refers to a ceramic microporous filter membrane with no wetting agent in the pores and full of penetrant. 3.2 Wet membrane
A ceramic microporous filter membrane fully infiltrated with a wetting agent is called a wet membrane. Main reagents and materials
The following reagents used in this method are all analytically pure. Pure water: in accordance with the technical indicators of GB17323. Solid NaOH.
-98% sulfuric acid.
Monoisobutyl alcohol.
Monoisopropyl alcohol.
Monomethyl red indicator: 0.1% methyl red indicator. Phenolic acid indicator: 1% phenolic acid indicator. 5 Instruments and equipment
Analytical balance: sensitivity 0.001g.
Industrial balance: maximum weighing 1kg, sensitivity 0.01g. Ultrasonic cleaning instrument.
Electric drying oven: (0～300)℃.
Approved by the State Oceanic Administration on 2002-12-30
Implementation on 2003-02-01
Dryer.
Material testing machine.
HY/T064—2002
Clamp, see Appendix A (Standard Appendix) Figure AI Bending strength test. Vernier caliper, accuracy 0.02mm.
Measurement device for pure water flux and maximum pore size, see Appendix A (Standard Appendix) Figure A2. Average pore size test device, see Appendix A (Standard Appendix) Figure A3. For the test device for acid and alkali corrosion resistance, see Figure A4 in Appendix A (Appendix to the standard). Conical flask and beaker, etc.
6 Test method
The test method for microporous membrane includes:
6.1 Pure water flux and maximum pore size test;
6.2 Average pore size test;
6.3 Porosity test;
6.4 Bending strength test;
6.5 Acid and alkali corrosion resistance test.
7 Inspection rules
7.1 Pure water flux and maximum pore size test
The pure water flux and maximum pore size measuring device are used for measurement, as shown in Figure A2 in Appendix A (Appendix to the standard). 7.1.1 Test and calculation of pure water flux
Pure water with conductivity less than 10μm·cm-1 and turbidity less than 0.1NTU is pressed through a ceramic microporous filter membrane at an operating pressure of 0.1MPa and a temperature of 25℃. The volume of pure water passing through the filter membrane per unit time and per unit membrane area is the pure water flux, which is calculated according to formula (1):
Wherein: F is the pure water flux of the membrane, m2·m-2·h-1; Q is the amount of pure water permeated through the membrane per unit time, m3·h-!; A is the effective membrane area, m2.
7.1.2 Maximum pore size test and calculation
First, the membrane is infiltrated with the selected impregnant, and nitrogen is used as the gas source. The pressure difference on both sides of the membrane is gradually increased, the minimum bubbling pressure is measured, and the maximum pore size is calculated.
Wherein: Dmax
The maximum pore size of the test membrane, m;
The surface tension of the solvent, N/m
The bubbling pressure difference, Pa.
7.2 Average pore size test
The average pore size test device is used for determination.
7.2.1 Principle
(2)
For ceramic microporous filter elements with different pore sizes, the gas exclusion method and the liquid-liquid exclusion method can be used for determination, as shown in Table 1. The gas exclusion method refers to the method of using gas to exclude the impregnant in the pores of the ceramic microporous filter membrane, and the average pore size is obtained by measuring the gas flow rate and the pressure difference on both sides of the membrane. The liquid-liquid exclusion rule is to replace the gas with another liquid that is immiscible with the infiltrating liquid and has a slightly lower wettability, so as to exclude the infiltrating liquid in the pores of the sample by measuring the flow rate of the liquid and the pressure difference on both sides of the membrane to obtain the average pore size. Table 1 Wetting agents and penetrants used in different pore size ranges Method
Gas exclusion method
Liquid-liquid exclusion method
Penetrating agent
Isobutanol-water saturated oil phase
The capillary action in the membrane pores is determined according to the Laplace equation: D. =
Where: D.———average pore size, μm; Wetting agent
Isobutanol
Isobutanol-water saturated water phase
△P. The pressure on both sides of the membrane corresponding to the time when the wet membrane flow rate is half of the dry membrane flow rate, MPa; a——interfacial tension between the two liquids, N/m. 7.2.2 Sample preparation
Glaze both ends of the ceramic microporous filter element to prevent the penetrant from penetrating from the end surface and affecting the test results. 7.2.3 Test method
7.2.3.1 Gas exclusion method test
Measurable pore size range/μm
0.2～0.05
0.05~0.004
(3)
a) Place the cleaned ceramic microporous filter test element in a 120℃ oven for 3 hours to remove moisture and other volatile components. b) Install the ceramic microporous filter membrane in a permeator. The structure of the permeator is shown in Figure B1 in Appendix B (Suggested Appendix). Use nitrogen as the gas source and gradually increase the pressure to make the nitrogen flow through the dry membrane. Measure the corresponding gas flux under different pressures and plot the membrane flow curve. c) Add the wetting agent to the permeabilizer cavity from the funnel and use a vacuum pump to suck until the entire permeabilizer is filled with the permeabilizer. Use nitrogen as the gas source and gradually increase the pressure to make the nitrogen flow through the wet membrane. Measure the corresponding gas flux under different pressures and draw a mixed membrane flow curve. d) When the wet membrane flow is half of the dry membrane flow, the corresponding pore size is the average pore size. 7.2.3.2 Liquid-liquid exclusion method
a) Place the cleaned ceramic microporous filter membrane test element in a 120℃ oven and bake for 2h~3h to remove moisture and other volatile components.
b) Add isobutanol-water saturated water phase to the permeator cavity from the funnel, and use a vacuum pump to suck so that the permeator is filled with the permeant. Add isobutanol-water saturated oil phase to the liquid storage tank, use nitrogen as the gas source, gradually increase the pressure, so that the isobutanol-water saturated oil phase flows through the water phase to infiltrate the wet membrane, accurately record the pressure difference and the corresponding flow value, and draw a graph to obtain the wet membrane flow curve. c) When the pressure rises to 0.7MPa, the membrane pores can be considered to be fully open. After removing the infiltrant on the permeation side, reduce the pressure and measure the permeate flow rate under different pressures. Draw a graph to obtain the dry membrane flow curve. d) When the wet membrane flow rate is half of the dry membrane flow rate, the corresponding pore size is the average pore size. 7.3 Porosity test
7.3.1 Preparation of test specimens
Take a test specimen from the middle and both ends of the test sample, and the length of each test specimen shall not be less than 25 mm. After the test specimen is ultrasonically cleaned with water for 5 minutes, it is placed in an electric drying oven and dried at 110°C to constant weight. It is taken out and placed in a desiccator, and weighed to an accuracy of 0.01 g. 7.3.2 Test steps
Operate according to the relevant details given in 5.2 of GB/T1966. 7.3.3 Calculation of results
Calculate according to the details given in Chapter 6 of GB/T1966. 7.4 Bending strength test
7.4.1 Preparation of test specimens
Cut 3 ceramic microporous filter membranes with a length of 120 mm. 3
7.4.2 Test steps
HY/T 064—2002
a) After the sample is ultrasonically cleaned with water for 5 minutes, it is placed in an electric heating drying oven and dried at 110℃ to constant weight, taken out and placed in a desiccator to cool to room temperature.
b) Adjust the distance between the supports to 100mm, place the sample on the supports, apply a load at a speed of 10N/s until the sample is destroyed, and read the load value F (N) at the time of destruction.
7.4.3 Data processing principles
The arithmetic mean of all samples is taken as the final result. 7.5 Acid and alkali corrosion resistance test
7.5.1 Preparation of samples
Cut 6 ceramic microporous filter membranes with a length of 120mm. 7.5.2 Test steps
a) Ultrasonic clean the sample with distilled water for 5 minutes; b) Dry at 110℃ for 2 hours, weigh, take 3 pieces each and place them in two 3000mL conical flasks; c) Add 2000mL of 20% sulfuric acid and 10% NaOH solution to the two conical flasks respectively; d) Install reflux condenser. Heat the solution and sample with an electric furnace with a voltage regulator and control them to reach a slightly boiling state within 20 minutes. Adjust the voltage, keep it at a slightly boiling state for 1 hour, and turn off the electric furnace; e) After cooling for 30 minutes, add 100mL of distilled water from the top of the condenser, remove the conical flask, pour out the liquid, take out the sample, place it in a sugar porcelain plate and rinse it with a large amount of water for 1 hour. After the indicator test shows neutrality, stop water rinsing; f) Dry at 110℃ for 2 hours and weigh accurately; g) Conduct bending strength test.
7.5.3 Calculation method
The mass loss rate of acid and alkali corrosion is calculated according to formula (4): Lm
Wherein: L.-mass loss rate, %;
ma—-mass of the specimen before corrosion, g;
mass after acid or alkali corrosion, g.
The strength loss rate of acid and alkali corrosion is calculated according to formula (5): mo
Wherein: Lt
Strength loss rate, %;
F---…strength of the specimen before corrosion, N;
strength after acid or alkali corrosion, N.
Take the average value as the final result.
8 Test report
The report should include the following contents:
.'a) Model of ceramic microporous filter membrane tested; b) Room temperature during test;
c) Test results;
d) Test date;
e) Operator and test unit.
(4)
HY/T064—2002
Appendix A
(Appendix of standard)
Test equipment
The test equipment used in the test is shown in Figures A1~A4. L=100
1—Upper loading blade; 2—Stainless steel fixture: 3—Test specimen; 4—Lower supporting blade Figure A1 Bending strength test figure
1—Pure water tank; 2—Stainless steel pump, 3—Pressure filter (0.2μm) 4—Permeabilizer; 5—Flow sensor; 6—Flow totalizer; 7~Pressure sensor; 8—Pressure display; 9—Separator; 10—Gas sensor; K0~K8—Stop valve; K9—Pressure regulating valve Figure A2 Test device for pure water flux and maximum pore size 5
HY/T064—2002
1-Nitrogen cylinder; 2-Liquid storage tank; 3-Permeator; 4-Recovery tank; 5-Precision pressure gauge; 6-Flowmeter Figure A3 Average pore size test device
1-Water outlet; 2-Iron stand; 3-Water inlet: 4-Conical bottle; 5-Electric furnace; 6-Pressure regulator Figure A4 Test device for acid and alkali corrosion resistance The structure of the permeator is shown in Figure B1.
HY/T064—2002
Appendix B
(Suggested Appendix)
Permeator structure diagram
Permeation side outlet
Sealing enclosure
Permeator2μm) 4-Permeator; 5-Flow sensor; 6-Flow integrator; 7~Pressure sensor; 8-Pressure display; 9-Separator; 10-Gas sensor; K0~K8-Stop valve; K9-Pressure regulating valve Figure A2 Pure water flux and maximum pore size test device 5
HY/T064—2002
1-Nitrogen cylinder; 2-Liquid storage tank; 3-Permeator; 4-Recovery tank; 5-Pressure gauge; 6-Flow meter Figure A3 Average pore size test device
1-Water outlet; 2-Iron frame; 3-Water inlet: 4 Conical flask; 5-Electric furnace; 6-Pressure regulator Figure A4 Acid and alkali corrosion resistance test device The structure of the permeator is shown in Figure B1.
HY/T064—2002
Appendix B
(Suggested Appendix)
Permeator Structure Diagram
Permeate Side OutletbZxz.net
Sealing Surrounding
Permeator2μm) 4-Permeator; 5-Flow sensor; 6-Flow integrator; 7~Pressure sensor; 8-Pressure display; 9-Separator; 10-Gas sensor; K0~K8-Stop valve; K9-Pressure regulating valve Figure A2 Pure water flux and maximum pore size test device 5
HY/T064—2002
1-Nitrogen cylinder; 2-Liquid storage tank; 3-Permeator; 4-Recovery tank; 5-Pressure gauge; 6-Flow meter Figure A3 Average pore size test device
1-Water outlet; 2-Iron frame; 3-Water inlet: 4 Conical flask; 5-Electric furnace; 6-Pressure regulator Figure A4 Acid and alkali corrosion resistance test device The structure of the permeator is shown in Figure B1.
HY/T064—2002
Appendix B
(Suggested Appendix)
Permeator Structure Diagram
Permeate Side Outlet
Sealing Surrounding
Permeator
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