CN109443996B - Device and method for sensitively detecting membrane permeation pressure value in membrane distillation process - Google Patents
Device and method for sensitively detecting membrane permeation pressure value in membrane distillation process Download PDFInfo
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- CN109443996B CN109443996B CN201811543492.3A CN201811543492A CN109443996B CN 109443996 B CN109443996 B CN 109443996B CN 201811543492 A CN201811543492 A CN 201811543492A CN 109443996 B CN109443996 B CN 109443996B
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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
Abstract
The invention discloses a device and a method for sensitively detecting membrane permeation pressure value in a membrane distillation process, wherein the device comprises a gas storage tank, a membrane permeation testing component, a direct-current power supply, a high-sensitivity electric bridge and a membrane to be tested; the membrane permeation testing assembly comprises an accommodating cylinder, a flange plate and a bottom plate, the membrane to be tested is positioned between the flange plate and the bottom plate, and a conducting strip is arranged between the membrane to be tested and the bottom plate; the gas storage tank is connected with the accommodating cylinder through a pressure reducing valve, a pressure regulator and a pressure gauge; an upper wiring terminal and a lower wiring terminal are further arranged at the upper end of the accommodating barrel and on the lower side of the conducting plate, and the direct-current power supply is connected with the upper wiring terminal and the lower wiring terminal; two wire columns are distributed on the side wall of the accommodating cylinder, and the high-sensitivity bridge is connected with the two wire columns; the method adopts the device to detect the membrane permeation pressure value. The invention can reflect the membrane wetting phenomenon through the electrical parameter detection of the membrane component, thereby rapidly and accurately indicating the maximum operation pressure which can be borne by the system.
Description
Technical Field
The invention relates to the technical field of membrane distillation separation, in particular to a device and a method for sensitively detecting membrane permeation pressure value in a membrane distillation process.
Background
Membrane distillation is a new low-energy consumption (such as thermal driving of waste heat and waste heat) water treatment process, and is a filtration and separation method based on a hydrophobic membrane material; the process principle is as follows (taking seawater desalination as an example): water molecules in feed liquid (located at the heating end of the membrane and in a high-temperature area) are heated and vaporized, and are driven by the partial pressure difference of steam on two sides of the membrane to migrate and permeate the membrane material in the form of steam, and the permeate liquid (located at the other end of the membrane and in a low-temperature area) is condensed and changed into liquid water. Ideally, the membrane material only allows vaporized molecules to permeate through, and can intercept any other materials existing in liquid state, so that the separation rate of the target material can reach as high as 99.99%. For example, water in seawater is converted into steam in the membrane distillation process and permeates through the membrane, while salt in seawater cannot be vaporized and still exists in the form of ions in the solution and cannot permeate through the membrane. Therefore, maintaining the "dryness" of the membrane material is a key guarantee for realizing efficient separation by the membrane distillation process.
However, in the existing membrane distillation process, dry membrane materials in the membrane distillation system are gradually soaked in the long-term application process, namely, liquid water molecules gradually enter membrane pores. In a wetted membrane pore, the liquid water will carry the dissolved material component through, resulting in zero material interception rate at the membrane pore. The membrane soaking phenomenon in the membrane distillation process is a gradual process which gradually begins from a tiny membrane hole (along the depth direction of the membrane hole) with time and gradually develops towards a local part, and finally, the whole membrane material is completely soaked. The membrane soaking threshold value is accurately detected as early as possible, so that the membrane soaking phenomenon is thoroughly avoided, and the method is very important for stable process operation and effluent quality guarantee. This requires accurate and sensitive detection of what pressure (vapor pressure driven by temperature difference) the liquid is initially subjected to as it enters the membrane pores.
Generally, the pore size of membrane materials varies, for example, the pore size distribution range of a membrane can be 0.01um to 0.5um, and under a certain operating pressure, the phenomenon of liquid entering the pores occurs preferentially in relatively large pores. The permeation phenomenon of the largest membrane pores in the membrane material must be accurately and quickly captured, and the real pressure threshold value which can be borne by the membrane can be accurately indicated. The large-scale device is adopted abroad, and the weight of the liquid is monitored in the process of continuously increasing the pressure, so that the liquid is indicated to enter a membrane hole and the phenomenon of permeation is indicated. The method cannot accurately and sensitively describe the soaking phenomenon in one or more membrane holes, so that the captured soaking phenomenon is delayed, namely the soaking threshold value (the driving pressure value of the membrane) is higher. If the operating pressure value measured in this way is used during the operation of the membrane distillation process, rapid membrane wetting will occur, resulting in failure of the entire membrane module.
Therefore, it is desirable to provide a device and a method for capturing the liquid "wet" phenomenon in a large pore channel or some membrane channels on the membrane material, so as to quickly and accurately indicate the maximum operation pressure that the system can bear.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to solve the technical problems in the prior art and provide a device and a method for sensitively detecting the membrane permeation pressure value in the membrane distillation process, which can reflect the membrane soaking phenomenon through the electrical parameter detection of a membrane component so as to sensitively capture the liquid permeation phenomenon in a large pore channel on a membrane material, thereby more sensitively and accurately capturing the operating pressure of a system when the maximum membrane pore on the membrane material is soaked with liquid; thereby rapidly and accurately indicating the maximum operation pressure which can be borne by the system.
In order to solve the technical problem, the technical scheme adopted by the invention is as follows: the utility model provides a device of sensitive detection membrane distillation in-process membrane soaks pressure value which characterized in that: the device comprises a gas storage tank, a membrane permeation testing component, a direct-current power supply, a high-sensitivity bridge and a membrane to be tested; the membrane permeation testing assembly comprises a containing cylinder made of metal materials, the upper end of the containing cylinder is closed, the lower end of the containing cylinder is open, and a bottom plate is used for sealing the lower end of the containing cylinder; a flange plate is sleeved at the lower end of the outer side of the accommodating cylinder, is made of metal and is fixedly connected with the accommodating cylinder; the bottom plate is made of an insulating material and is connected with the flange plate through a connecting bolt; the membrane to be tested is positioned between the flange plate and the bottom plate and seals the lower end of the containing cylinder; a conducting strip is arranged between the membrane to be tested and the bottom plate, and the membrane to be tested separates the conducting strip from the flange plate and the lower end of the accommodating cylinder;
the upper end of the accommodating barrel is provided with a liquid injection port and an air inlet, the liquid injection port is used for injecting electrolyte solution into the accommodating barrel, and an air outlet of the air storage tank is connected with the air inlet at the upper end of the accommodating barrel after passing through a pressure reducing valve, a pressure regulator and a pressure gauge; an upper binding post and a lower binding post are respectively arranged at the upper end of the accommodating barrel and at the lower side of the conducting strip, the upper end of the lower binding post is fixedly connected with the conducting strip, and the lower side of the lower binding post penetrates through the bottom plate; the positive pole of the direct current power supply is connected with the upper wiring terminal, and the negative pole of the direct current power supply is connected with the lower wiring terminal;
two wire columns are further distributed on the side wall of the accommodating cylinder up and down, and the positive electrode and the negative electrode of the high-sensitivity bridge are respectively connected with the two wire columns.
Furthermore, an O-shaped sealing ring is arranged between the membrane to be measured and the flange plate.
Further, the conducting sheet is a graphite sheet or a copper sheet.
Furthermore, on the bottom plate, a through hole is formed in the position corresponding to the lower wiring column, and the lower end of the lower wiring column penetrates through the through hole.
Further, the gas filled in the gas storage tank is nitrogen.
Further, the high-sensitivity bridge adopts a multimeter.
A method for sensitively detecting the membrane permeation pressure value in the membrane distillation process is characterized in that: the apparatus of any preceding claim, comprising the steps of:
1) mounting a membrane to be tested on a membrane saturation test assembly;
2) injecting electrolyte solution into the accommodating barrel through the liquid injection port until the electrolyte solution fills the space between the accommodating barrel and the membrane to be tested;
3) connecting a direct current power supply, and supplying power to the membrane penetration testing assembly through the direct current power supply;
4) opening a valve of the gas storage tank and a pressure reducing valve;
5) adjusting the pressure regulator to gradually increase the air pressure in 5kPa increments, wherein each pressure value lasts for 30 s;
6) observing the high-sensitivity electric bridge, and recording the reading of the pressure gauge when the displayed electric parameters of the high-sensitivity electric bridge obviously fluctuate; the reading is the maximum operation pressure value which can be borne by a membrane in the membrane distillation system;
7) repeating steps 1) -6) a plurality of times to verify the pressure value measured in step 6).
Further, the electrolyte solution is a 20% NaCl solution.
Further, the electrical parameter is an electrical impedance, a capacitance or a voltage.
Further, when the fluctuation of the electrical parameter is 10% or more, the fluctuation is regarded as significant.
Compared with the prior art, the invention has the following advantages:
1. the device has the advantages of simple structure, small occupied space, simple structure and simple and convenient operation.
2. The device is simple to operate, can detect and reflect the membrane soaking phenomenon through the electrical parameters of the membrane component so as to sensitively capture the liquid soaking phenomenon in a large pore channel on the membrane material, thereby more sensitively and accurately capturing the operating pressure of the system when the maximum membrane pore on the membrane (material) is soaked with the liquid; thereby rapidly and accurately indicating the maximum operation pressure which can be borne by the system.
3. The device has stable performance and good repeatability, and can ensure the accuracy and credibility of experimental results.
4. The device adopts the electrical parameters of the membrane component as response parameters to detect the membrane soaking phenomenon for the first time, has high sensitivity and innovation, and the response parameter values are convenient to observe and record.
5. The detection method has the advantage of wide range of membrane pore testing, and can sensitively and rapidly detect the membrane pore soaking with the pore size distribution of 0.01-0.5 um on the membrane.
6. The detection method is simple and rapid, and can rapidly detect the operating pressure of the system when the maximum membrane hole on the membrane (material) is soaked with liquid, thereby greatly improving the detection efficiency.
7. The detection method has the advantages of low cost and low investment, and various accessories required in the device are convenient and easy to obtain.
8. The detection method has the advantage of high yield, the detection result of the operating pressure of the system when the maximum membrane pores on the membrane (material) are soaked with liquid can greatly improve the accuracy of the high-efficiency separation of the membrane distillation experiment, the stable operation of the process is facilitated, the quality of effluent water can be ensured to a certain extent, and the experiment failure caused by the soaking of the membrane component in the experiment operation process is avoided.
Drawings
FIG. 1 is a schematic view of the apparatus of the present invention.
FIG. 2 is a schematic diagram of the membrane permeation test assembly of the present invention.
In the figure: the device comprises a gas storage tank 1, a membrane soaking test component 2, a direct current power supply 3, a high-sensitivity bridge 4, a diaphragm to be tested 5, a containing cylinder 6, a flange 7, a bottom plate 8, a conducting strip 9, a liquid injection port 10, an air inlet 11, a pressure reducing valve 12, a pressure regulator 13, a pressure gauge 14, an upper wiring terminal 15, a lower wiring terminal 16, a wire guiding column 17 and an O-shaped sealing ring 18.
Detailed Description
The invention will be further explained with reference to the drawings and the embodiments.
Example (b): referring to fig. 1 and 2, the device for sensitively detecting the membrane permeation pressure value in the membrane distillation process comprises an air storage tank 1, a membrane permeation testing component 2, a direct current power supply 3, a high-sensitivity bridge 4 and a membrane 5 to be tested. The membrane permeation test assembly 2 comprises a containing cylinder made of metal materials with the upper end closed and the lower end opened and a bottom plate 8 with the lower end closed. A flange 6 is sleeved at the lower end of the outer side of the accommodating cylinder, and the flange 6 is made of metal and is fixedly connected with the accommodating cylinder; the flange plate 6 and the accommodating cylinder are made of metal materials, so that the conductive performance is good, and the detection of electrical parameters in the detection process is facilitated. In actual processing, the flange 6 and the accommodating cylinder are formed into a whole, and the lower side surface of the flange 6 is flush with the lower end surface of the accommodating cylinder; in this way, the mounting of the membrane 5 to be tested is facilitated.
The bottom plate 8 is made of an insulating material and is connected with the flange plate 6 through a connecting bolt; the membrane 5 to be measured is positioned between the flange 6 and the bottom plate 8, and the lower end of the containing cylinder is closed. A conducting strip 9 is arranged between the membrane 5 to be measured and the bottom plate 8, and the membrane 5 to be measured separates the conducting strip 9 from the flange 6 and the lower end of the containing cylinder. Like this, because the diaphragm 5 that awaits measuring is insulating material usually, separate holding bucket and ring flange 6 and conducting strip 9 through the diaphragm 5 that awaits measuring to can effectively avoid conducting strip 9 directly to electrically conduct. During specific implementation, an O-shaped sealing ring 18 is further arranged between the membrane 5 to be detected and the flange plate 6, so that the problem that the solution in the accommodating cylinder leaks to influence the detection accuracy and stability can be avoided. Wherein, the conducting strip 9 is a graphite sheet or a copper sheet; the conductivity is better, and the cost is lower.
The upper end of the accommodating barrel is provided with a liquid injection port 10 and an air inlet 11, and the liquid injection port 10 is used for injecting electrolyte solution into the accommodating barrel; an air outlet of the air storage tank 1 is connected with an air inlet 11 at the upper end of the containing cylinder through a pressure reducing valve 12, a pressure regulator 13 and a pressure gauge 14. The gas filled in the gas storage tank 1 is nitrogen; because nitrogen is inert gas and is not easy to react with the solution, the nitrogen is adopted for pressurization, the influence on the detection result can be avoided, and the accuracy of the detection result is higher. An upper wiring terminal 15 and a lower wiring column 16 are respectively arranged at the upper end of the accommodating barrel and at the lower side of the conducting strip 9, the upper end of the lower wiring column 16 is fixedly connected with the conducting strip 9, and the lower side penetrates through the bottom plate 8. In the actual processing process, on bottom plate 8, the position that corresponds post 16 is equipped with the via hole down, the lower extreme of post 16 passes from this via hole down, and like this, the assembly is convenient more, swift. The positive pole of the direct current power supply 3 is connected with the upper binding post 15, and the negative pole is connected with the lower binding post 16.
Two wire columns 17 are also distributed on the side wall of the accommodating cylinder up and down, and the positive and negative poles of the high-sensitivity bridge 4 are respectively connected with the two wire columns 17. In specific implementation, the high-sensitivity bridge 4 adopts a (high-sensitivity) multimeter, so that the operation is simple, and the reading is accurate and convenient.
In the detection process, a method of pressurizing the membrane permeation test component 2 by using a gas storage tank 1 (nitrogen tank) as a pressure source; the pressure of the pressurization is controlled by a pressure reducing valve 12, fine-tuned by a pressure regulator 13, and read by a pressure gauge 14. Electrolyte is filled in the membrane permeation test component 2, a membrane 5 to be tested is placed at the sealing position below the membrane permeation test component 2, and a conducting strip 9 is placed below the membrane 5 to be tested. Thus, the sealed membrane permeation test assembly 2 filled with the electrolyte is pressurized, when the membrane surface pressure reaches the value that the electrolyte can penetrate through the membrane 5 to be tested and is in contact with the conducting strip 9, if the high-sensitivity bridge 4 additionally arranged on the membrane permeation test assembly 2 displays that the electrical parameters (electrical impedance, capacitance and voltage) of the membrane permeation test assembly 2 have obvious fluctuation (the data range is more than or equal to 10%), the solution permeation phenomenon in the largest membrane hole is indicated. Accordingly, the test circuit is now completed (the membrane pores are filled with a high-concentration salt solution which is a good conductor and after soaking the pores are conductive). The membrane permeation pressure value is obtained by recording the reading of the pressure gauge 14 at this time.
The device has a simple structure, can detect and reflect the membrane soaking phenomenon through the electrical parameters of the membrane component so as to sensitively capture the liquid soaking phenomenon in a large pore channel on the membrane material, thereby more sensitively and accurately capturing the operating pressure of the system when the maximum membrane pore on the membrane (material) is soaked with the liquid; thereby rapidly and accurately indicating the maximum operation pressure which can be borne by the system.
A method for sensitively detecting the membrane permeation pressure value in the membrane distillation process utilizes the device, and comprises the following specific steps:
1) the membrane 5 to be tested is mounted on the membrane saturation test assembly 2.
2) Electrolyte solution is injected into the accommodating barrel through the liquid injection port 10 until the electrolyte solution fills the space between the accommodating barrel and the diaphragm 5 to be measured. Wherein the electrolyte solution is a NaCl solution with the concentration of 20%; the conductivity is better, can detect the state that the membrane soaks fast, accurately.
3) The direct current power supply 3 is switched on, and the membrane permeation test assembly 2 is powered through the direct current power supply 3; since the electrolyte solution does not permeate from the membrane 5 to be tested at this time, the membrane permeation test assembly 2 is in an open circuit state, and thus the data detected by the high-sensitivity bridge 4 is zero or very small.
4) The valve of the air storage tank 1 and the pressure reducing valve 12 are opened.
5) The pressure regulator 13 is adjusted to gradually increase the air pressure in 5kPa increments, wherein each pressure value lasts 30 s.
6) Observing the high-sensitivity bridge 4, and recording the reading of the pressure gauge 14 at the moment when the displayed electrical parameter obviously fluctuates; the reading is the maximum operation pressure value which can be borne by a membrane in the membrane distillation system; wherein the electrical parameter is electrical impedance, capacitance or voltage. When the electrical parameter fluctuation is 10% or more, it is regarded as a significant fluctuation. When the membrane 5 to be tested permeates, the electrolyte solution is in contact with the conducting strip 9, at the moment, the whole membrane permeation test assembly 2 is in a conduction state, the electrical parameter in the power-on state can be detected through the high-sensitivity bridge 4, and the value of the electrical parameter is usually far larger than that of the electrical parameter detected in the circuit breaking state.
7) Repeating steps 1) -6) a plurality of times to verify the pressure value measured in step 6).
The method is simple and rapid, and can rapidly detect the operating pressure of the system when the maximum membrane hole on the membrane (material) is soaked with liquid, thereby greatly improving the detection efficiency.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting the technical solutions, and those skilled in the art should understand that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all that should be covered by the claims of the present invention.
Claims (7)
1. A method for sensitively detecting the membrane permeation pressure value in the membrane distillation process is characterized in that: the device comprises a gas storage tank, a membrane permeation testing component, a direct-current power supply, a high-sensitivity bridge and a membrane to be tested; the membrane permeation testing assembly comprises a containing cylinder made of metal materials, the upper end of the containing cylinder is closed, the lower end of the containing cylinder is open, and a bottom plate is used for sealing the lower end of the containing cylinder; a flange plate is sleeved at the lower end of the outer side of the accommodating cylinder, is made of metal and is fixedly connected with the accommodating cylinder; the bottom plate is made of an insulating material and is connected with the flange plate through a connecting bolt; the membrane to be tested is positioned between the flange plate and the bottom plate and seals the lower end of the containing cylinder; a conducting strip is arranged between the membrane to be tested and the bottom plate, and the membrane to be tested separates the conducting strip from the flange plate and the lower end of the accommodating cylinder; the upper end of the accommodating barrel is provided with an injection port and an air inlet, the injection port is used for injecting electrolyte solution into the accommodating barrel, gas filled in the gas storage tank is nitrogen, and an air outlet of the gas storage tank is connected with the air inlet at the upper end of the accommodating barrel after passing through a pressure reducing valve, a pressure regulator and a pressure gauge; an upper binding post and a lower binding post are respectively arranged at the upper end of the accommodating barrel and at the lower side of the conducting strip, the upper end of the lower binding post is fixedly connected with the conducting strip, and the lower side of the lower binding post penetrates through the bottom plate; the positive pole of the direct current power supply is connected with the upper wiring terminal, and the negative pole of the direct current power supply is connected with the lower wiring terminal; a through hole is formed in the bottom plate at a position corresponding to the lower wiring column, and the lower end of the lower wiring column penetrates through the through hole; two wire columns are also distributed on the side wall of the accommodating cylinder up and down, and the positive and negative poles of the high-sensitivity bridge are respectively connected with the two wire columns;
the method comprises the following specific steps:
1) mounting a membrane to be tested on a membrane saturation test assembly;
2) injecting electrolyte solution into the accommodating barrel through the liquid injection port until the electrolyte solution fills the space between the accommodating barrel and the membrane to be tested;
3) connecting a direct current power supply, and supplying power to the membrane penetration testing assembly through the direct current power supply;
4) opening a valve of the gas storage tank and a pressure reducing valve;
5) adjusting the pressure regulator to gradually increase the air pressure in 5kPa increments, wherein each pressure value lasts for 30 s;
6) observing the high-sensitivity electric bridge, and recording the reading of the pressure gauge when the displayed electric parameters of the high-sensitivity electric bridge obviously fluctuate; the reading is the maximum operation pressure value which can be borne by a membrane in the membrane distillation system;
7) repeating steps 1) -6) a plurality of times to verify the pressure value measured in step 6).
2. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: an O-shaped sealing ring is arranged between the membrane to be measured and the flange plate.
3. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: the conducting strip is a graphite sheet or a copper sheet.
4. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: the high-sensitivity electric bridge adopts a universal meter.
5. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: the electrolyte solution is a NaCl solution with the concentration of 20 percent.
6. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: the electrical parameter is electrical impedance, capacitance or voltage.
7. The method for sensitively detecting the membrane permeation pressure value in the membrane distillation process as claimed in claim 1, wherein: and when the electric parameter fluctuation is more than or equal to 10%, the electric parameter is regarded as obvious fluctuation.
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