CN114618321B - Hollow fiber membrane, preparation and application thereof in hydraulic oil degassing - Google Patents
Hollow fiber membrane, preparation and application thereof in hydraulic oil degassing Download PDFInfo
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- CN114618321B CN114618321B CN202011458475.7A CN202011458475A CN114618321B CN 114618321 B CN114618321 B CN 114618321B CN 202011458475 A CN202011458475 A CN 202011458475A CN 114618321 B CN114618321 B CN 114618321B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D19/00—Degasification of liquids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/58—Other polymers having nitrogen in the main chain, with or without oxygen or carbon only
- B01D71/62—Polycondensates having nitrogen-containing heterocyclic rings in the main chain
- B01D71/64—Polyimides; Polyamide-imides; Polyester-imides; Polyamide acids or similar polyimide precursors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/66—Polymers having sulfur in the main chain, with or without nitrogen, oxygen or carbon only
- B01D71/68—Polysulfones; Polyethersulfones
Abstract
The invention provides a preparation and modification method of a hollow fiber membrane for removing dissolved air in aviation hydraulic oil, the prepared hollow fiber membrane has excellent tolerance to hydraulic oil, stable performance in high-pressure hydraulic oil and no phenomenon of penetration in a hydraulic oil film and swelling of the membrane. In the process of degassing the hydraulic oil by a membrane method, the hydraulic oil flows outside the membrane, and osmotic power is formed on the inner side of the membrane by vacuumizing, so that air dissolved in the hydraulic oil permeates through the membrane and is effectively removed. The preparation and modification method of the hollow fiber membrane provided by the invention can effectively improve the removal efficiency and process reliability of dissolved air in hydraulic oil, and simultaneously can greatly improve the contact area of the hydraulic oil and a degassing membrane by controlling the size of the hollow fiber membrane and working in the form of a hollow fiber membrane assembly, and has the advantages of high degassing efficiency, low energy consumption, small critical volume requirement on an aviation system and the like.
Description
Technical field:
the invention relates to a preparation and modification method of a hollow fiber membrane for hydraulic oil degassing, belonging to the technical fields of functional membranes and aviation safety.
The background technology is as follows:
the hydraulic transmission is widely applied in the aerospace field due to the characteristics of large power-to-volume ratio, easy automation realization and the like. The hydraulic system is an important secondary energy system of the aircraft, oil is used as a working medium, and the hydraulic driving actuating mechanism is used for completing specific maneuvering actions such as retraction and extension of the landing gear, braking, turning, flight control, thrust reverser, cabin door maneuvering and the like. The working medium of the hydraulic system of the modern passenger plane is flame-retardant phosphate-based hydraulic oil. The data show that 50-70% of failures in the use of the hydraulic system are caused by pollution of the hydraulic system. The improvement of the control accuracy requirements of the hydraulic system of the airplane also puts higher demands on the pollution control level of the working medium. Generally, the control technology of solid particle pollutants and liquid pollution in hydraulic oil is mature at present, but the control research of air pollution is still lacking.
In fact, the air pollution in hydraulic systems has a very serious effect on their performance, mainly expressed in the following aspects: (1) reducing the oil volume modulus: the existence of free gas in the oil liquid can greatly reduce the elastic modulus of the oil liquid, so that the system is slow in response and unstable in operation, and poor aircraft maneuvering following performance is caused; (2) cavitation: when oil enters high pressure from low pressure, bubbles are instantaneously compressed and destroyed to generate local high-temperature and high-pressure impact, so that damage is caused to hydraulic elements; (3) cause system pressure instability: the existence of gas in the oil liquid influences the stability of the operating force of the system, and the bubble precipitation can cause the fluctuation of the pressure of the system, so that the condition of incomplete operation is generated; (4) increasing the system temperature rise: when a large amount of free gas is compressed sharply, local high temperature is generated, even sparks are generated, and oil liquid can be burnt and carbonized; (5) promoting the oxidative deterioration of oil liquid: the increase of the air content in the oil inevitably causes oxidation corrosion to the oil, increases the acid value of the oil and shortens the service life of the oil; (6) generating noise and vibration: the air contained in the oil liquid frequently dissolves and precipitates along with the change of the pressure, and noise and vibration which are difficult to eliminate are formed in the system.
Air pollution in hydraulic oils is mainly caused by two reasons: the external air is directly dissolved in the hydraulic oil (open oil tank) when contacting with the hydraulic oil, and the air pollution is generated in the running process of the system. Despite the various precautions taken in hydraulic system design, air pollution is still difficult to avoid completely, and there is evidence that even closed systems, which still contain 25% of dissolved air, need to be removed, so constant removal of air during operation is very important for proper operation of the hydraulic system. The exhaust means adopted at present mainly comprise exhaust valve exhaust, centrifugal exhaust, vacuum exhaust and the like.
Chinese patent CN92108634.2 provides a method for degassing and dewatering from oil, comprising the input of oil to be treated, vacuum degassing, dewatering and the output of treated oil, characterized in that the oil is subjected to a throttling step before entering the vacuum tank.
Chinese patent CN202010532953.8 provides a defoaming device, which comprises a tank body, and is characterized in that a partition board is arranged in the tank body, the partition board divides the tank body into an upper tank cavity and a lower tank cavity, a swirl port for conducting the upper tank cavity and the lower tank cavity is arranged on the partition board, and the liquid level of hydraulic oil in the tank body is higher than the height of the partition board; the lower cavity of the oil tank is internally provided with a swirl cavity through an arc swirl plate, hydraulic oil injected into the lower cavity of the oil tank forms swirl through the swirl cavity and separates out light hydraulic oil containing bubbles, and the light hydraulic oil is converged into the upper cavity of the oil tank through a swirl port.
The method is complex in operation, the regularity, uniformity, reliability and the like of exhaust cannot be guaranteed, and aiming at the hydraulic oil degassing requirement of a civil aircraft, the invention provides a method for removing dissolved air in a hydraulic system by adopting the prepared hollow fiber membrane. Membrane technology is widely used in the field of gas separation and has proven to be an efficient and reliable process. The gas permeates through the polymer in a "dissolution diffusion" manner under the driving force of the pressure difference, while the hydraulic oil cannot permeate through the membrane due to the larger molecular volume/hydrophilic rejection of the membrane surface, etc. According to the technical background, a hollow fiber membrane component is added in a return pipeline of a hydraulic system, hydraulic oil flows through a shell layer of the component, the inner tube of the membrane is in a vacuum state, so that component pressure difference is formed at two sides of the membrane, under the action of the pushing force, air dissolved in the hydraulic oil permeates through the membrane, the amount of the dissolved air in the axial hydraulic oil flowing direction of the hollow fiber membrane is gradually reduced along with the progress of the degassing process, and finally, the high-efficiency removal of the dissolved air in the hydraulic system is realized.
Based on the background, the invention provides a preparation and modification method of a hollow fiber membrane for removing dissolved air in aviation hydraulic oil.
Disclosure of Invention
Aiming at the fact that a large amount of dissolved air exists in the aviation hydraulic oil, which forms a great challenge for the safe flight of an aircraft, the invention is urgently required to develop objective requirements for safely, reliably and stably realizing the degassing process of the hydraulic oil, and provides the preparation and modification method of the hollow fiber membrane, which can have excellent tolerance to the hydraulic oil, has stable performance in high-pressure hydraulic oil and has no obvious swelling and hydraulic oil film inner penetration phenomena in the hydraulic oil, from the aspect of improving the stability and high efficiency of the membrane in the degassing process of the hydraulic oil.
The preparation method comprises the steps of firstly, dissolving a specific high polymer material with stable performance in hydraulic oil by adopting a mixed solvent to prepare uniform membrane liquid, and finely regulating and controlling a phase conversion process by changing spinning process parameters to prepare a hollow fiber membrane bottom membrane with a compact and defect-free cortex structure or a hollow fiber membrane with epidermis defect holes; the former has a dense skin thickness, so the gas flux is small but can be directly applied to the hydraulic oil degassing process; the latter has a thin dense skin layer and defective holes, so that the gas flux is high, but the high-pressure hydraulic oil can penetrate through the membrane and cannot be directly applied, and the high-pressure hydraulic oil can be applied to the degassing process of the hydraulic oil after the surface defective holes are subjected to sealing modification treatment by adopting specific materials.
The specific steps of the invention are as follows:
A. preparing a casting film liquid: mixing and stirring the polymer/solvent/non-solvent in a certain proportion at 50-90 ℃ to form a uniform solution, and vacuum defoaming to prepare a transparent casting film solution with the polymer content of 25-35 wt%;
the membrane material can be polyimide, polyetherimide, polysulfone, polyethersulfone, polyphenylsulfone, polyvinylidene fluoride, cellulose, polyacetyl cellulose and the like; the solvent can be N-methylpyrrolidone, dimethylacetamide, dimethyl sulfoxide, dioxane, cyclohexanone, tetrahydrofuran, etc.; the non-solvent can be methanol, ethanol, acetone, water, butyrolactone, etc.;
B. the hollow fiber membrane is prepared by adopting an immersion phase inversion method and dry-wet spinning, and the spinning process parameters are as follows: spinning temperature is 50-110 ℃, dry spinning distance is 0-500 mm, external gel bath is tap water with 0-50 ℃, internal core liquid is aqueous solution containing 0-90 wt% solvent, and 100-500 KPa of N is applied to a film liquid tank 2 Pushing the membrane liquid into a gear pump, accurately controlling the flow by the gear pump, extruding the membrane liquid into a gel bath through a spray head, and forming a hollow fiber bottom membrane under the combined action of the inner gel bath and the outer gel bath;
C. washing the hollow fiber membrane with flowing tap water for more than 48 hours to fully wash off residual solvent in the membrane, then adopting a solvent replacement method (ethanol is used for replacing water in the membrane and n-hexane is used for replacing ethanol) to fully remove water in the membrane, putting the bottom membrane into a vacuum oven with the temperature of 50-120 ℃ for drying after n-hexane is volatilized, and obtaining the hollow fiber membrane bottom membrane with a compact and defect-free cortex structure or the hollow fiber membrane with the epidermis defect holes according to different initial concentration of membrane liquid;
the specific spinning process flow comprises the following steps: the spinning solution is extruded out of the spinning solution tank by compressed nitrogen, metered by a metering pump, enters a filter, then enters a cavity between an inner pipe and an outer pipe of a cannula type spinning nozzle, and enters a gel bath after passing through an air layer dry spinning stage with a certain height after being extruded. The core liquid is controlled by a horizontal pump to be pressed into an inner pipe of a spray head from a storage container, and the spray head is extruded with spinning solution at the same time, so that the spinning solution enters a gel bath to be solidified into primary fibers after passing through a dry spinning stage, a hollow fiber membrane is washed by flowing tap water for more than 48 hours to sufficiently wash off residual solvent in the membrane, and then a solvent replacement method (ethanol is adopted to replace water in the membrane and n-hexane is adopted to replace ethanol) is adopted to sufficiently remove water in the membrane; after n-hexane volatilizes, putting the bottom film into a vacuum oven with the temperature of 50-120 ℃ for drying for 2-5 hours to obtain a dry hollow fiber film;
D. the method for plugging and modifying the surface hole defect of the hollow fiber membrane is characterized in that firstly, the hollow fiber membrane is prepared into a membrane component with a suitable specification, a coating liquid with the concentration of 1-10wt% is prepared, polymers adopted by the coating can be cellulose acetate, polyethylene glycol, chitosan, polyvinyl alcohol, polylactic acid and the like, and certain cross-linking agents, generally glutaraldehyde and boric acid, are added into the coating liquid according to different directions of the polymers; the prepared coating liquid is placed on the outer side of a hollow fiber membrane in a membrane assembly, power is formed in a mode of vacuumizing the inner side of the membrane, so that the coating liquid enters the membrane holes, and the coating liquid is prevented from entering the hollow holes of the membrane through the defect holes by regulating the vacuum degree; the redundant coating liquid outside the membrane is removed under the condition that the hollow side is kept under vacuum, and the method can be water washing, ethanol washing, methanol washing and the like; then placing the assembly into a vacuum oven with the temperature set to be 50-100 ℃ for high-temperature crosslinking modification treatment; the surface hole defect of the membrane component treated by the process can be effectively removed, and the method can be applied to the hydraulic oil degassing process.
The hollow fiber membrane prepared by the invention has excellent tolerance to hydraulic oil, stable performance in high-pressure hydraulic oil and no phenomenon of penetration in a hydraulic oil film and swelling of the membrane. In the process of degassing the hydraulic oil by a membrane method, the hydraulic oil flows outside the membrane, and osmotic power is formed on the inner side of the membrane by vacuumizing, so that air dissolved in the hydraulic oil permeates through the membrane and is effectively removed. The preparation and modification method of the hollow fiber membrane provided by the invention can effectively improve the removal efficiency and process reliability of dissolved air in hydraulic oil, and simultaneously can greatly improve the contact area of the hydraulic oil and a degassing membrane by controlling the size of the hollow fiber membrane and working in the form of a hollow fiber membrane assembly, and has the advantages of high degassing efficiency, low energy consumption, small critical volume requirement on an aviation system and the like.
Compared with the common hydraulic oil degassing device and process, the invention has the following advantages:
(1) The membrane method is adopted to carry out the degassing process on the hydraulic oil, so that the hydraulic oil is simple, stable and reliable;
(2) The membrane method degassing principle is based on the permeation rate of gas in the membrane, and the degassing uniformity and efficiency are high;
(3) The hollow fiber membrane has small size and high specific surface, and can provide an ultrahigh degassing area for hydraulic oil degassing;
(4) The hollow fiber membrane component has small volume and does not cause volume burden on an aviation hydraulic oil degassing system;
(5) The specification of the membrane component is variable, and a proper membrane component can be selected according to specific degassing requirements, so that the adaptability is high.
Based on the summary, the preparation and modification method of the hollow fiber membrane for removing dissolved air in the aviation hydraulic oil provided by the invention has important value in realizing the efficient degassing process of the aviation system hydraulic oil in China.
Drawings
FIG. 1 is a hollow fiber membrane electron micrograph;
FIG. 2 is a schematic illustration of a hollow fiber membrane module for use in a hydraulic oil degassing process, wherein: 1, an epoxy seal head; 2 hollow fiber membranes; 3 hydraulic oil inlet (not degassed); 4/6 of the removed air outlet (negative pressure); 5 hydraulic oil outlet (after degassing), the whole size of the assembly is a cylinder with the diameter of 8.0cm and the length of 20.0cm, wherein the total number of hollow fiber membranes is 33000. The assembly was installed in the return line of the hydraulic system to remove the amount of dissolved air contained in 140L of hydraulic oil from 25% to a level of 5% within 1 hr.
Detailed Description
Example 1
36 g of polyimide is added into 64 g of mixed solvent of NMP/tetrahydrofuran (weight ratio is 6:1), stirred for 24 hours under the protection of nitrogen at 90 ℃ to be completely dissolved, and after vacuum defoamation, the casting solution with the concentration of 36 weight percent is obtained and then is put into a spinning tank for wet spinning. The spinning temperature was 70℃and the core liquid was 95wt% NMP in water at a flow rate of 0.4ml/min, the gel bath was water and the water bath temperature was room temperature. The hollow fiber membrane was dried by solvent displacement method after washing in flowing deionized water for 24 hours (ethanol was first used to displace water in the membrane, then n-hexane was used to displace ethanol, and after n-hexane was volatilized, the base membrane was dried in a vacuum oven at 80 ℃ for 6 hours). Scanning electron microscopy revealed that the hollow fiber membrane had a dense defect-free cortical structure (as in fig. 1).
The inner/outer diameter of the carrier film was 0.36mm/0.18mm. The gas permeation rate of the prepared carrier film was measured. O of the polyimide film at 25℃and 0.5MPa 2 Penetration rate was 12.0GPU (1gpu=10 -6 cm 3 (STP)/(cm 2 ·s·cmHg))，N 2 Is 2.0GPU. The oxygen-nitrogen separation coefficient is 6.0, which is equivalent to the intrinsic oxygen-nitrogen separation coefficient of polyimide material, and shows that the prepared hollow fiber membrane cortex has no defective pores and can be directly applied to the hydraulic oil degassing process.
Example 2
Immersing the hollow fiber membrane described in example 1 in hydraulic oil for 60 days, wherein the membrane has no swelling phenomenon; the hollow fiber membrane is prepared into a component, hydraulic oil is introduced into the outer side of the membrane, the pressure is increased to 3.0MPa, continuous pressure application is carried out for 30 days, and no hydraulic oil permeation phenomenon exists in the membrane, so that the prepared polyimide hollow fiber membrane has excellent hydraulic oil tolerance.
Example 3
The hollow fiber membrane bundle described in example 1 was prepared as a degassing membrane module shown in fig. 2, and when the degassing treatment of the hydraulic oil was performed, the hydraulic oil was passed through the outer side of the membrane filaments and the inner side was subjected to the evacuation treatment (vacuum degree 90 KPa).
The degassing membrane component comprises a closed hollow cylinder, the left end and the right end of the cylinder are respectively provided with a gas outlet, two partition boards are respectively arranged in the cylinder near the left end and the right end and are respectively provided with a gas outlet, and the peripheral edges of the partition boards are in closed connection with the inner wall surface of the cylinder; the separator separates the inside of the cylinder into a left chamber, a middle chamber and a right chamber which are not communicated with each other, the hollow fiber membrane is arranged in the middle chamber of the cylinder, the two ends of the hollow fiber membrane penetrate through the separator and respectively extend out of the left chamber and the right chamber, and a material inlet and a material outlet are arranged on the wall surface of the middle chamber.
Claims (4)
1. The application of the hollow fiber membrane in hydraulic oil degassing is that the preparation method of the hollow fiber membrane comprises the following specific steps:
1) Preparing a casting film liquid: mixing and stirring the polymer, the solvent and the non-solvent at 50-90 ℃ to form a uniform solution, and carrying out vacuum defoaming to prepare a casting solution with the polymer content of 20-40 wt%;
the polymer can be more than one of polyimide, polyetherimide, polysulfone, polyethersulfone, polyphenylsulfone, polyvinylidene fluoride, cellulose and cellulose acetate; the solvent can be one or more of N-methylpyrrolidone (NMP), dimethylacetamide, dimethyl sulfoxide, dioxane, cyclohexanone and tetrahydrofuran; the non-solvent can be more than one of methanol, ethanol, acetone, water and butyrolactone;
the weight ratio of the solvent to the non-solvent is determined according to the phase diagram of the casting film system and the spinning requirement, and the weight ratio of the solvent to the non-solvent is 4:1 to 19:1, adjusting;
2) The hollow fiber membrane is prepared by adopting an immersion phase inversion method and dry-wet spinning, and the spinning process parameters are as follows: spinning temperature is 50-110 ℃, dry spinning distance is 0-500 mm, outer gel bath is 0-50 ℃ water, inner tube core liquid is aqueous solution containing 0-95 wt% solvent;
the casting solution is extruded into a gel bath through a spray head, and hollow fiber membranes are formed under the combined action of the inner gel bath and the outer gel bath;
the solvent of the inner tube core liquid is more than one of N-methyl pyrrolidone, dimethylacetamide, dimethyl sulfoxide, dioxane, cyclohexanone and tetrahydrofuran; a method for plugging and modifying surface hole defects of a hollow fiber membrane,
1) Firstly, preparing a hollow fiber membrane into a hollow fiber membrane component, and preparing a coating liquid with the concentration of 1-10wt%, wherein the polymer adopted by the coating can be more than one of cellulose acetate, polyethylene glycol, chitosan, polyvinyl alcohol and polylactic acid, and the cross-linking agent is one or two of glutaraldehyde and boric acid;
the hollow fiber membrane component comprises a hollow closed container, wherein the hollow fiber membrane is arranged in the container, two ends of the hollow fiber membrane penetrate through the wall surface of the container and extend out of the container, and a material inlet and a material outlet are arranged on the wall surface of the container;
2) The prepared coating liquid is placed in a container of a membrane assembly and outside a hollow fiber membrane, power is formed by vacuumizing the inner side of the hollow fiber membrane, so that the coating liquid enters membrane holes, and the coating liquid is prevented from entering the hollow holes of the membrane through defect holes by regulating the vacuum degree;
3) The method for removing the excessive coating liquid outside the hollow fiber membrane under the condition of keeping vacuum inside the hollow fiber membrane can be one or more of water washing, ethanol washing and methanol washing;
4) Then placing the assembly into a vacuum oven with the temperature set to be 50-100 ℃ for high-temperature crosslinking modification treatment; the surface hole defect of the membrane component treated by the process can be effectively removed;
washing the hollow fiber membrane prepared by adopting a submerged phase inversion method for at least 24 hours by flowing tap water to sufficiently wash away residual solvent in the membrane, then sufficiently removing water in the membrane by adopting a solvent replacement method, replacing water in the membrane by ethanol firstly, replacing the ethanol by normal hexane, and drying the hollow fiber membrane in a vacuum oven with the temperature of 50-120 ℃ after the normal hexane volatilizes;
according to different initial concentrations of the casting solution, the high-concentration casting solution can prepare a hollow fiber membrane bottom membrane with a compact and defect-free cortex structure, and the low-concentration casting solution can prepare a hollow fiber membrane with epidermis defect holes;
the high concentration is casting film liquid with the polymer content of 30 wt% -40 wt%;
the low concentration is polymer content of 20-wt% -30 wt%, and does not contain 30 wt% of casting solution;
the hollow fiber membrane with the epidermis defect holes is used for measuring the permeation rate of oxygen and nitrogen, and the separation coefficient of the oxygen and the nitrogen is obviously lower than the intrinsic oxygen-nitrogen separation coefficient of the material; the hollow fiber membrane is subjected to hole blocking and modification methods, and defective holes on the surface of the hollow fiber membrane are subjected to complete sealing treatment.
2. The use according to claim 1, characterized in that:
applying 100-500 KPa N to a casting film liquid tank 2 The membrane liquid is pushed to enter the gear pump, the flow is accurately controlled by the gear pump, the membrane casting liquid is extruded into the gel bath through the spray head, and the hollow fiber membrane is formed under the combined action of the inner gel bath and the outer gel bath.
3. The use according to claim 1, characterized in that:
the outer side of the membrane is provided with a compact and defect-free cortex structure; the membrane is used for measuring the permeation rate of oxygen and nitrogen, and the separation coefficient of the oxygen and the nitrogen can reach and exceed the intrinsic oxygen-nitrogen separation coefficient of the material.
4. The use according to claim 1, characterized in that:
the hollow fiber membrane has no swelling in hydraulic oil, and can realize the property that the hydraulic oil cannot permeate through the membrane.
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