Preparation device and preparation process of hollow fiber membrane substrate for oil-gas separation

Abstract

The invention discloses a preparation device and a preparation process of a hollow fiber membrane substrate for oil-gas separation. The device comprises an extrusion forming unit, a phase conversion membrane forming unit and a filament collecting and cleaning unit, the extrusion forming unit comprises a membrane casting liquid extrusion pump, a core liquid extrusion pump, a constant-temperature circulating water machine, a spinning head and a spinning head position control system, and is used for carrying out defoaming treatment on a membrane casting liquid and a core liquid and extruding the membrane casting liquid and the core liquid; the phase conversion membrane forming unit comprises a spinning cavity and a coagulation tank and is used for performing water-gas induced phase separation and non-solvent induced phase separation on the membrane casting liquid and the core liquid to form a formed hollow fiber membrane matrix; and the filament collecting and washing unit is used for collecting and washing filaments of the formed hollow fiber membrane matrix to obtain the hollow fiber membrane matrix. The hollow fiber membrane is prepared by combining a non-solvent induced phase separation method with a water-gas induced phase separation method, meanwhile, process parameters of all units are controlled, continuous production of the hollow fiber membrane is achieved, the automation degree is high, and the parameters can be accurately controlled.

Description

Technical Field

[0001] The invention relates to the field of preparation of hollow fiber membrane substrates for oil-gas separation, and in particular to a hollow fiber membrane substrate preparation device for oil-gas separation and a preparation process thereof. Background Art

[0002] The hollow fiber membrane used for oil-gas separation is mainly composed of a matrix and a functional layer. The functional layer mainly plays the role of separating gas from oil, and the matrix mainly plays a supporting role and a role of gas permeation. Therefore, the matrix needs to meet the requirements of low surface pore size, small surface pore distribution, high porosity, and excellent chemical, mechanical and thermal stability. At present, the commonly used materials for hollow fibers are ceramic materials and polymer materials. Compared with ceramic materials, polymer materials have a lower unit price, strong processability, and are easy to prepare in large quantities to reduce production costs.

[0003] The preparation methods of the polymer matrix of the oil-gas separation composite membrane usually adopt non-solvent induced phase separation (NIPS), thermal induced phase transition (TIPS) and vapor induced phase separation (VIPS). The non-solvent induced phase separation (NIPS) method is that the polymer solution is in a non-solvent of a constant temperature system, and the mass transfer exchange between the solvent and the non-solvent is used to allow the non-solvent to extract the solvent in the polymer solution, so that the concentration of the polymer solution is increased to cause phase separation, and finally solidify into a film matrix. The thermal induced phase transition method (TIPS) uses the temperature change of the system to reduce the solubility of the homogeneous polymer solution and cause the polymer to undergo phase transition behavior. In the process, the polymer solution is mainly converted from a liquid state to a gelled state, and finally solidified from the gelled state into a film matrix. The vapor-induced phase separation method (VIPS) is to dissolve the polymer in a solvent with a high boiling point and good affinity for water, then expose the polymer solution to different humidity environments. The solvent has a good affinity for water and absorbs water vapor into the polymer solution, causing the composition of the polymer solution to change and cause phase separation, and finally solidify into a film matrix.

[0004] At present, non-solvent induced phase separation (NIPS) and thermal induced phase transition (TIPS) are widely used. Chinese patent CN213132683U proposes a PVDF hollow fiber membrane preparation device using non-solvent induced phase separation (NIPS), but the rapid exchange of non-solvent and solvent during the preparation process of this method easily causes the hollow fiber membrane to form a finger-like pore structure, and the porosity of the outer surface is low, and the separation performance and mechanical properties are poor. Chinese patents CN102000515A and CN104857864A both use thermal induced phase transition (TIPS) to prepare hollow fiber membranes, so that the pores on the membrane surface are more and more evenly distributed, effectively improving the membrane structure and greatly improving the membrane performance, but the phase separation speed is too fast, which will lead to the formation of closed pores and other problems. In addition, the device has poor controllability and is prone to bubbles, causing discontinuous production. Chinese patent CN116726717A proposes a continuous membrane preparation method that integrates a non-solvent induced phase separation method (NIPS) with a vapor induced phase separation method (VIPS). This method can delay the phase separation process and the mass transfer rate is relatively slow, so that a honeycomb pore structure can be formed inside the membrane, so that it meets the requirements of the oil-soluble gas composite membrane matrix. However, this patent is suitable for the preparation of flat membranes, not for hollow fiber membranes. Summary of the invention

[0005] In order to solve the deficiencies in the prior art, the present invention proposes a hollow fiber membrane substrate preparation device for oil and gas separation and a preparation process thereof. The device can realize the preparation of hollow fiber membrane substrates by combining non-solvent induced phase separation (NIPS) with vapor induced phase separation (VIPS), and can accurately control the process parameters and environmental control parameters of each step, which is conducive to efficiently regulating the macro and micro structures of the hollow fiber membrane substrate. The device has an automated control system and can continuously prepare hollow fiber membrane substrates for oil and gas separation.

[0006] The present invention adopts the following technical solution.

[0007] The first aspect of the present invention discloses a hollow fiber membrane substrate preparation device for oil-gas separation, comprising an extrusion molding unit, a phase conversion membrane unit and a fiber collection and cleaning unit connected in sequence;

[0008] The extrusion molding unit comprises a casting liquid extrusion pump, a core liquid extrusion pump, a constant temperature circulating water machine and a spinning head. The casting liquid extrusion pump and the core liquid extrusion pump are respectively connected to the constant temperature circulating water machine, and the constant temperature circulating water machine is used to defoam the casting liquid and the core liquid; the casting liquid extrusion pump and the core liquid extrusion pump extrude the casting liquid and the core liquid at a fixed rate and enter the spinning head;

[0009] The phase conversion membrane unit comprises a spinning chamber and a condensation tank, the spinning chamber is arranged above the condensation tank, the spinning head in the extrusion molding unit is arranged inside the spinning chamber, the casting liquid and the core liquid undergo a water vapor induced phase separation and a non-solvent induced phase separation process in the phase conversion membrane unit to form a molded hollow fiber membrane matrix;

[0010] The fiber collecting and cleaning unit collects and washes the hollow fiber membrane matrix formed in the phase conversion membrane unit to obtain the hollow fiber membrane matrix.

[0011] Preferably, the casting film liquid extrusion pump comprises a casting film liquid extrusion pump temperature control layer and a casting film liquid extrusion pump controller, and the casting film liquid extrusion pump temperature control layer is arranged outside the casting film liquid extrusion pump controller; the core liquid extrusion pump comprises a core liquid extrusion pump temperature control layer and a core liquid extrusion pump controller, and the core liquid extrusion pump temperature control layer is arranged outside the core liquid extrusion pump controller;

[0012] The circulating water pipeline of the constant temperature circulating water machine is connected with the temperature control layer of the film casting liquid extrusion pump and the temperature control layer of the core liquid extrusion pump, so that the constant temperature circulating water flows through the film casting liquid extrusion pump and the core liquid extrusion pump to control the temperature of the solution in the extrusion pump and remove the bubbles in the added solution;

[0013] The casting liquid extrusion pump controller is used to control the casting liquid to be extruded from the spinning head at a constant rate and a fixed speed, and the core liquid extrusion pump controller is used to control the core liquid to be extruded from the spinning head at a constant rate and a fixed speed.

[0014] Preferably, the spinning head comprises a spinning head casting liquid inlet interface and a spinning head core liquid inlet interface; the casting liquid extrusion outlet of the casting liquid extrusion pump is connected to the spinning head casting liquid inlet interface; the core liquid extrusion outlet of the core liquid extrusion pump is connected to the spinning head core liquid inlet interface.

[0015] Preferably, the extrusion molding unit also includes a lifting mechanism, which includes: a screw, a spinning head clamping rod, a tension rotating motor and a limit switch. The spinning head clamping rod clamps the spinning head, and the tension rotating motor is connected to the screw for driving the screw to rotate. The spinning head clamping rod is threadedly connected to the screw. When the tension rotating motor drives the screw to rotate, the spinning head clamping rod performs a lifting movement along the axial direction of the screw.

[0016] Preferably, the outside of the spinning chamber is provided with a micro refrigeration compressor, an evaporator, a condenser and an air conveying motor which are connected in sequence, and the outlets thereof are all connected to the spinning chamber for controlling the temperature and humidity inside the spinning chamber.

[0017] Preferably, a baffle with telescopic holes is provided at the lower part of the spinning chamber, and the telescopic holes of the baffle are correspondingly arranged on the same straight line as the extrusion holes of the spinning head.

[0018] Preferably, a first pumping motor is installed outside the condensation tank, and the outlet of the first pumping motor is connected to the inlet at the bottom of the condensation tank;

[0019] A first positioning roller, a condensation tank heating tube and a condensation tank temperature sensor are arranged inside the condensation tank, the condensation tank heating tube is arranged at the bottom of the condensation tank, and the condensation tank temperature sensor is arranged on one side inner wall of the condensation tank; a second positioning roller is arranged at the upper part of the tail end of the condensation tank;

[0020] The first positioning roller and the second positioning roller are cooperatively connected with the wire collecting and cleaning unit.

[0021] Preferably, a third positioning roller and a wire guide are arranged on the upper part of the wire collecting and cleaning unit, and the third positioning roller and the wire guide are cooperatively connected with the second positioning roller; a wire collecting roller with a motor is arranged inside the wire collecting and cleaning unit, and a second water-pumping motor is arranged outside the wire collecting and cleaning unit, and the wire collecting roller is cooperatively connected with the wire guide; the outlet of the second water-pumping motor is connected to the bottom inlet of the wire collecting and cleaning unit.

[0022] Preferably, a controller is further included, the wire guide machine includes a wire guide screw, and the controller is electrically connected to the wire guide screw and is used to control the movement of the wire guide screw to adjust the wire collection position of the hollow fiber membrane.

[0023] Preferably, a controller is also included, which is electrically connected to the pulling rotation motor and the limit switch respectively, and is used to control the spinning head clamping rod in the lifting mechanism to move to a preset position.

[0024] The second aspect of the present invention discloses a process for preparing a hollow fiber membrane substrate for oil-gas separation, based on the device for preparing a hollow fiber membrane substrate for oil-gas separation, comprising the following steps:

[0025] Under a preset temperature environment, the casting liquid and the core liquid are subjected to defoaming treatment for a preset time respectively;

[0026] The casting liquid and the core liquid are squeezed and water-gas induced phase separation is performed simultaneously to obtain a primary hollow fiber membrane;

[0027] Inducing phase separation in a non-solvent environment to form a hollow fiber membrane;

[0028] Clean the hollow fiber membrane.

[0029] Preferably, the casting solution is any one of a polyamide-imide / N-methylpyrrolidone solution, a polyvinylidene fluoride / N-methylpyrrolidone solution, a polyamide-imide / dimethyl sulfoxide solution, a polyvinylidene fluoride / dimethyl sulfoxide solution, a polysulfone / N-methylpyrrolidone solution, and a polysulfone / dimethyl sulfoxide solution;

[0030] The concentration of the casting solution is 15-30wt%.

[0031] Preferably, the core liquid is one or more of N-methylpyrrolidone, dimethylformamide, dimethylacetamide or dimethyl sulfoxide;

[0032] The core liquid is diluted with deionized water, and the mass percentage of the deionized water is 5-35wt%.

[0033] Compared with the prior art, the beneficial effects of the present invention include at least:

[0034] (1) The hollow fiber membrane substrate preparation device and preparation process for oil-gas separation proposed in the present invention realizes the simultaneous use of water vapor induced phase separation (VIPS) and non-solvent induced phase separation (NIPS) to prepare the hollow fiber membrane by setting an extrusion molding unit and a phase conversion membrane unit. The present invention uses an extrusion pump controller and a constant temperature circulating water machine to control the process parameters of each unit, maintain a stable separation speed, remove bubbles, and effectively realize the continuous production of the hollow fiber membrane;

[0035] (2) The hollow fiber membrane prepared by the hollow fiber membrane substrate preparation device and preparation process for oil-gas separation proposed in the present invention has an outer diameter of 0.7-1.0 mm, an inner diameter of 0.4-0.7 mm, and a wall thickness of 0.15-0.3 mm, which can be used as a substrate material for oil-gas separation membranes and can achieve continuous spinning;

[0036] (3) The hollow fiber membrane substrate preparation device for oil-gas separation proposed in the present invention has a high degree of automation, and the parameters can be precisely controlled through an interactive interface. The microstructure of the hollow fiber membrane can be regulated by adjusting the process parameters. BRIEF DESCRIPTION OF THE DRAWINGS

[0037] Figure 1 A schematic structural diagram of a hollow fiber membrane substrate preparation device for oil-gas separation according to an embodiment of the present invention is shown;

[0038] Figure 2 A schematic structural diagram of a spinning head in a hollow fiber membrane substrate preparation device for oil-gas separation according to an embodiment of the present invention is shown;

[0039] In the figure: 101. casting liquid extrusion pump, 1011. casting liquid extrusion pump temperature control layer, 1012. casting liquid extrusion pump controller, 102. core liquid extrusion pump, 1021. core liquid extrusion pump temperature control layer, 1022. core liquid extrusion pump controller, 103. constant temperature circulating water machine, 104. spinning head, 1041. spinning head casting liquid inlet interface, 1042. spinning head core liquid inlet interface, 105. lifting mechanism, 1051. screw, 1052. spinning head clamping rod, 1053. pulling force rotation motor, 1054. limit switch, 201. spinning chamber, 2 011. Micro refrigeration compressor, 2012. Evaporator, 2013. Condenser, 2014. Air conveying motor, 2015. Temperature and humidity sensor, 2016. Heating tube, 2017. Baffle, 202. Coagulation groove, 2021. First water pumping motor, 2022. First positioning roller, 2023. Coagulation groove heating tube, 2024. Coagulation groove temperature sensor, 2025. Second positioning roller, 301. Wire collection and cleaning unit, 3011. Third positioning roller, 3012. Wire guide machine, 3013. Wire collection roller, 3014. Second water pumping motor. DETAILED DESCRIPTION

[0040] In order to make the purpose, technical scheme and advantages of the present invention clearer, the technical scheme of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. The embodiments described in this application are only embodiments of a part of the present invention, rather than all embodiments. Based on the spirit of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative work belong to the protection scope of the present invention.

[0041] like Figure 1 and Figure 2 As shown, Example 1 of the present invention discloses a hollow fiber membrane substrate preparation device for oil-gas separation, including an extrusion molding unit, a phase conversion membrane unit and a fiber collection and cleaning unit 301.

[0042] The extrusion molding unit is used to defoam the casting liquid and the core liquid, and extrude the casting liquid and the core liquid from the spinning head at a constant speed and a fixed quantity, and can control the air gap length. It includes a casting liquid extrusion pump 101, a core liquid extrusion pump 102, a constant temperature circulating water machine 103, a spinning head 104 and a lifting mechanism 105. The casting liquid extrusion pump 101 and the core liquid extrusion pump 102 are respectively connected to the constant temperature circulating water machine 103, the casting liquid extrusion pump 101 is connected to the spinning head 104, and the spinning head 104 is connected to the lifting mechanism 105.

[0043] The casting film liquid extrusion pump 101 includes a casting film liquid extrusion pump temperature control layer 1011 and a casting film liquid extrusion pump controller 1012, and the casting film liquid extrusion pump temperature control layer 1011 is arranged outside the casting film liquid extrusion pump controller 1012; the core liquid extrusion pump 102 includes a core liquid extrusion pump temperature control layer 1021 and a core liquid extrusion pump controller 1022, and the core liquid extrusion pump temperature control layer 1021 is arranged outside the core liquid extrusion pump controller 1022;

[0044] The circulating water pipeline of the constant temperature circulating water machine 103 is connected to the external circulating water temperature control layer 1011 of the casting liquid extrusion pump and the external circulating water temperature control layer 1021 of the core liquid extrusion pump, so that the constant temperature circulating water flows through the casting liquid extrusion pump 101 and the core liquid extrusion pump 102 to control the temperature of the solution in the extrusion pump, remove the bubbles in the added solution, prevent the hollow fiber membrane from defects, and control the temperature of the solution during the preparation process to ensure the controllable preparation conditions. The temperature control range is 10-90°C.

[0045] The casting liquid extrusion pump 101 is connected to the spinning head 104; specifically, the spinning head 104 includes a spinning head casting liquid inlet interface 1041 and a spinning head core liquid inlet interface 1042, and the casting liquid extrusion outlet of the casting liquid extrusion pump 101 is connected to the spinning head casting liquid inlet interface 1041 through a stainless steel pipe, and the casting liquid is squeezed out of the outer hole of the spinning head by accurately controlling the extrusion speed through the casting liquid extrusion pump controller 1012.

[0046] The core liquid extrusion outlet of the core liquid extrusion pump 102 is connected to the core liquid inlet interface 1042 of the spinning head through stainless steel, and the core liquid extrusion pump controller 1022 accurately controls the extrusion speed to squeeze the core liquid out of the inner hole of the spinning head.

[0047] Both the casting liquid extrusion pump 101 and the core liquid extrusion pump 102 are equipped with filters to filter impurities in the solution, thereby ensuring the quality of film formation and improving the product qualification rate.

[0048] The lifting mechanism 105 includes a screw 1051, a spinning head clamping rod 1052, a pulling force rotating motor 1053 and a limit switch 1054. The spinning head clamping rod 1052 clamps the spinning head 104, and a height and level detector is installed on the upper part to adjust its level and height position. The level detector is used to observe whether it is in a horizontal position. The pulling force rotating motor 1053 is connected to the screw 1051 for driving the screw 1051 to rotate. The spinning head clamping rod 1052 is threadedly connected to the screw 1051. When the pulling force rotating motor 1053 drives the screw 1051 to rotate, the spinning head clamping rod 1052 performs a lifting movement along the axial direction of the screw 1051. After the height is set by the controller, the spinning head is automatically adjusted to the corresponding height to control the air distance. The limit switch 1054 is located inside the housing of the lifting mechanism 105, at the highest point that the spinning head clamping rod can reach, and is used to limit the position of the spinning head clamping rod to prevent exceeding the range.

[0049] The phase conversion membrane unit is a membrane unit in which the casting liquid and the core liquid extruded from the spinning head 104 undergo water vapor induced phase separation and non-solvent induced phase separation to form a shaped hollow fiber membrane matrix, which includes a spinning chamber 201 and a condensation groove 202, and the spinning chamber 201 is arranged above the condensation groove 202.

[0050] The spinning chamber 201 has a metal and glass shell and a heat-insulating layer; the outside of the spinning chamber is provided with a micro-refrigeration compressor 2011, an evaporator 2012, a condenser 2013 and an air-moving motor 2014 which are connected in sequence, and the outlets thereof are all connected to the inside of the spinning chamber 201; the inside of the spinning chamber 201 is provided with a temperature and humidity sensor 2015 and a heating tube 2016; the lower part of the spinning chamber 201 is provided with a baffle 2017 with a telescopic hole.

[0051] The coagulation tank 202 is provided with a first pumping motor 2021 on the outside, and its water outlet is connected to the bottom inlet of the coagulation tank 202; the coagulation tank 202 is provided with a first positioning roller 2022, a coagulation tank heating pipe 2023 and a coagulation tank temperature sensor 2024; the coagulation tank heating pipe 2023 is provided at the bottom of the coagulation tank 202, and the coagulation tank temperature sensor 2024 is provided on one side inner wall of the coagulation tank 202;

[0052] A second positioning roller 2025 is disposed at the upper portion of the tail end of the condensation groove 202 , and the first positioning roller 2022 and the second positioning roller 2025 are connected to the wire collecting and cleaning unit 301 , and the formed hollow fiber membrane is connected to the second positioning roller 2025 through transmission, so that the formed hollow fiber membrane enters the wire collecting and cleaning unit 301 .

[0053] The micro refrigeration compressor 2011, evaporator 2012, condenser 2013, air motor 2014, temperature and humidity sensor 2015 and heating tube 2016 can intelligently control the temperature and humidity of the spinning chamber 201. The casting liquid and core liquid are squeezed out from the spinning head and undergo water vapor induced phase separation in the spinning chamber to form a primary hollow fiber membrane, thereby delaying the phase separation process and forming honeycomb pores.

[0054] The nascent hollow fiber membrane is pulled through a baffle 2017 with a telescopic hole and enters a coagulation tank filled with a non-solvent. After non-solvent-induced phase separation, a shaped hollow fiber membrane is formed. The shaped hollow fiber membrane bypasses the first positioning roller 2022, the second positioning roller 2025, the third positioning roller 3011 and the wire guide machine 3012, and is wound on the wire collection roller 3013. The wire collection roller 3013 can be speed-controlled by a motor to achieve the winding of the hollow fiber membrane. At the same time, the second water pumping motor 3014 continuously circulates deionized water in the wire collection cleaning unit to clean and remove residual solvent.

[0055] The wire collecting and cleaning unit 301 collects the formed hollow fiber membrane substrate and rinses the solvent with deionized water to obtain the hollow fiber membrane substrate, on the upper part of which a third positioning roller 3011 and a wire guide machine 3012 are arranged, and the third positioning roller 3011 and the wire guide machine 3012 are connected with the second positioning roller 2025; a wire collecting roller 3013 with a motor is arranged inside, and a second water-pumping motor 3014 is arranged outside, and the wire collecting roller 3013 is connected with the wire guide machine 3012; the outlet of the second water-pumping motor 3014 is connected with the bottom inlet of the wire collecting and cleaning unit 301.

[0056] In a preferred but non-limiting embodiment of the present invention, after the preparation is completed, the casting liquid extrusion pump 101 is cleaned with the corresponding pure solvent in the casting liquid, and the non-solvent in the condensation tank 202 is replaced to remove the residual casting liquid and non-solvent in the preparation process, thereby increasing the service life of the device.

[0057] Furthermore, the extrusion volume of the casting liquid extrusion pump 101 and the core liquid extrusion pump 102 is 0-500mL, the extrusion pressure range is 0.7-258.6bar, the extrusion rate range is 0.001-200mL / min, the displacement resolution is 31.71nL, and the filtration pore size is 0.5μm. The corresponding parameters are set through the interactive interface, the extrusion rate of the casting liquid and the core liquid can be precisely controlled, and the pressure in the pump at the corresponding extrusion rate can be accurately recorded through the pressure sensor, which is beneficial to control the macro and micro structure of the membrane.

[0058] Furthermore, the spinning head 104 can be selected in different sizes, with an outer diameter ranging from 1 to 3 mm and an inner diameter ranging from 0.5 to 1.5 mm, so as to prepare hollow fiber membranes of different sizes.

[0059] Furthermore, the height of the spinning head 104 is set through the interactive interface, and the clamping rod 1052 automatically reaches the corresponding position. The controller is electrically connected to the tension rotation motor 1053 and the limit switch 1054 respectively. The height of the spinning head 104 can be controlled in the range of 0-100 cm to control the air distance length of the water vapor induced phase separation, thereby adjusting the prepared hollow fiber membrane microstructure.

[0060] Furthermore, the baffle 2017 has a retractable small hole, which is arranged opposite to the extrusion hole of the spinning head 104 and located on the same straight line, so that the nascent hollow fiber membrane can enter the condensation groove, and other positions can separate the condensation groove from the spinning cavity to control the temperature and humidity in the spinning cavity, so as to ensure higher precision control of the temperature and humidity in the spinning cavity. The diameter of the retractable hole of the baffle is in the range of 0.5-10 cm.

[0061] The temperature control range in the spinning chamber 201 is 10-90°C, and the humidity control range is 10-90%RH. It has an intelligent temperature and humidity control system, and can be automatically adjusted by setting corresponding values ​​in the system.

[0062] Furthermore, the coagulation tank 202 has a heating tube 2023 and a temperature sensor 2024, which can control the temperature range to 25-90°C, and has an intelligent temperature control system. By setting the corresponding value of the system, it can be automatically adjusted to meet the temperature control of the non-solvent induced phase separation process.

[0063] Furthermore, the wire guide machine 3012 has a wire guide screw, a wire guide drive plate and a wire guide electromechanical control box. The controller is electrically connected to the wire guide screw. The wire collection position of the hollow fiber membrane is automatically controlled by setting the interactive interface setting value of the wire guide electromechanical control box to ensure that the hollow fiber can be laid flat on the wire collection roller and the hollow fiber membrane is cleaned. The movable range of the wire guide machine is 0-60cm.

[0064] Furthermore, a second pumping motor 3014 is installed outside the wire collection and cleaning unit to circulate deionized water to ensure that the residual solvent in the hollow fiber membrane is rinsed clean.

[0065] Furthermore, the wire collection speed range of the wire collection roller 3013 is 0-200m / h, and the wire collection speed can be precisely controlled to wind the hollow fiber membrane on the wire collection roller.

[0066] According to experiments, the hollow fiber membrane prepared by the hollow fiber membrane substrate preparation device for oil and gas separation has an outer diameter of 0.7-1.0mm, an inner diameter of 0.4-0.7mm, and a wall thickness of 0.15-0.3mm. It can be used as a substrate material for oil and gas separation membranes and can achieve continuous spinning.

[0067] According to Example 1 of the present invention, Example 2 of the present invention proposes a process for preparing a hollow fiber membrane substrate for oil-gas separation, and the process is as follows:

[0068] Under a preset temperature environment, the casting liquid and the core liquid are subjected to defoaming treatment for a preset time respectively;

[0069] The casting liquid and the core liquid are squeezed and water-gas induced phase separation is performed simultaneously to obtain a primary hollow fiber membrane;

[0070] Inducing phase separation in a non-solvent environment to form a hollow fiber membrane;

[0071] Clean the hollow fiber membrane.

[0072] In a preferred but non-limiting embodiment of the present invention, the preparation process specifically comprises the following steps:

[0073] S1, adding the casting liquid and the core liquid into the casting liquid extrusion pump and the core liquid extrusion pump respectively, starting the constant temperature circulating water machine to control the casting liquid extrusion pump and the core liquid extrusion pump at 60-80° C. for 4-24 hours, and defoaming the casting liquid and the core liquid;

[0074] Specifically, the casting solution includes but is not limited to polyamide-imide (PAI) / N-methylpyrrolidone (NMP) solution, polyvinylidene fluoride (PVDF) / N-methylpyrrolidone (NMP) solution, polyamide-imide (PAI) / dimethyl sulfoxide (DMSO) solution, polyvinylidene fluoride (PVDF) / dimethyl sulfoxide (DMSO) solution, polysulfone (PSF) / N-methylpyrrolidone (NMP) solution, polysulfone (PSF) / dimethyl sulfoxide (DMSO) solution, and the solution concentration is 15-30wt%.

[0075] Specifically, the core liquid includes but is not limited to one or a mixed solvent of N-methylpyrrolidone, dimethylformamide, dimethylacetamide or dimethyl sulfoxide, and is diluted with deionized water, and the mass percentage of deionized water is 5-35wt%.

[0076] S2, lowering the temperature of the constant temperature circulating water machine to the required control temperature, controlling the temperature and humidity in the spinning chamber to the set values ​​through the intelligent temperature and humidity control system, filling the condensation tank with non-solvent, controlling the temperature to the set value through the intelligent temperature control system of the condensation tank, adding deionized water to the collection and cleaning unit and circulating it continuously;

[0077] Specifically, the temperature control range of the constant temperature circulating water machine, the spinning chamber, and the coagulation tank is 25-70° C., the humidity control range of the spinning chamber is 20-90% RH, and deionized water is used as the non-solvent.

[0078] S3, installing the spinning head on the spinning clamping rod, adjusting the height and level of the spinning head, starting the casting liquid extrusion pump and the core liquid extrusion pump, so that the casting liquid and the core liquid are squeezed out of the spinning head, and performing water-gas induced phase separation in the spinning cavity to obtain a primary hollow fiber membrane;

[0079] Specifically, the height of the spinning head from the non-solvent horizontal plane is controlled in the range of 10-90 cm.

[0080] Specifically, the extrusion rate control range of the casting liquid extrusion pump is 1-5 ml / min, and the extrusion rate control range of the core liquid extrusion pump is 0.5-2 ml / min.

[0081] S4, the newly formed hollow fiber membrane enters the coagulation tank and undergoes non-solvent induced phase separation to form a shaped hollow fiber membrane, and the hollow fiber membrane is wound on the wire collection roller through three positioning rollers and a wire guide machine, and the hollow fiber membrane is further cleaned in the wire collection cleaning unit;

[0082] Specifically, the wire collection speed of the wire collection roller ranges from 0 to 200 m / h.

[0083] S5, after the preparation is completed, the casting liquid extrusion pump is cleaned with a solvent and the non-solvent in the coagulation tank is replaced.

[0084] Compared with the prior art, the beneficial effects of the present invention include at least:

[0085] (1) The hollow fiber membrane substrate preparation device and preparation process for oil-gas separation proposed in the present invention realizes the simultaneous use of water vapor induced phase separation (VIPS) and non-solvent induced phase separation (NIPS) to prepare the hollow fiber membrane by setting an extrusion molding unit and a phase conversion membrane unit. The present invention uses an extrusion pump controller and a constant temperature circulating water machine to control the process parameters of each unit, maintain a stable separation speed, remove bubbles, and effectively realize the continuous production of the hollow fiber membrane;

[0086] (2) The hollow fiber membrane prepared by the hollow fiber membrane substrate preparation device and preparation process for oil-gas separation proposed in the present invention has an outer diameter of 0.7-1.0 mm, an inner diameter of 0.4-0.7 mm, and a wall thickness of 0.15-0.3 mm, which can be used as a substrate material for oil-gas separation membranes and can achieve continuous spinning;

[0087] (3) The hollow fiber membrane substrate preparation device for oil-gas separation proposed in the present invention has a high degree of automation, and the parameters can be precisely controlled through an interactive interface. The microstructure of the hollow fiber membrane can be regulated by adjusting the process parameters.

[0088] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention rather than to limit it. Although the present invention has been described in detail with reference to the above embodiments, ordinary technicians in the relevant field should understand that the specific implementation methods of the present invention can still be modified or replaced by equivalents, and any modifications or equivalent replacements that do not depart from the spirit and scope of the present invention should be covered within the scope of protection of the claims of the present invention.

Claims

1. A hollow fiber membrane substrate preparation device for oil-gas separation, characterized in that: It comprises an extrusion molding unit, a phase conversion film unit and a wire collection and cleaning unit (301) which are connected in sequence; The extrusion molding unit comprises a casting liquid extrusion pump (101), a core liquid extrusion pump (102), a constant temperature circulating water machine (103) and a spinning head (104); the casting liquid extrusion pump (101) and the core liquid extrusion pump (102) are respectively connected to the constant temperature circulating water machine (103); the constant temperature circulating water machine (103) is used to perform defoaming treatment on the casting liquid and the core liquid; the casting liquid extrusion pump (101) and the core liquid extrusion pump (102) extrude the casting liquid and the core liquid at a fixed rate and into the spinning head (104); The phase conversion membrane unit comprises a spinning chamber (201) and a condensation tank (202), the spinning chamber (201) is arranged above the condensation tank (202), the spinning head (104) in the extrusion molding unit is arranged inside the spinning chamber (201), and the casting liquid and the core liquid undergo a water vapor induced phase separation and a non-solvent induced phase separation process in the phase conversion membrane unit to form a molded hollow fiber membrane matrix; The fiber collecting and cleaning unit (301) collects and washes the hollow fiber membrane matrix formed in the phase conversion membrane unit to obtain the hollow fiber membrane matrix.

2. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: The casting liquid extrusion pump (101) comprises a casting liquid extrusion pump temperature control layer (1011) and a casting liquid extrusion pump controller (1012), wherein the casting liquid extrusion pump temperature control layer (1011) is arranged outside the casting liquid extrusion pump controller (1012); the core liquid extrusion pump (102) comprises a core liquid extrusion pump temperature control layer (1021) and a core liquid extrusion pump controller (1022), wherein the core liquid extrusion pump temperature control layer (1021) is arranged outside the core liquid extrusion pump controller (1022); The circulating water pipeline of the constant temperature circulating water machine (103) is connected to the temperature control layer (1011) of the film casting liquid extrusion pump and the temperature control layer (1021) of the core liquid extrusion pump, so that the constant temperature circulating water flows through the film casting liquid extrusion pump (101) and the core liquid extrusion pump (102) to control the temperature of the solution in the extrusion pump and remove bubbles in the added solution; The casting liquid extrusion pump controller (1012) is used to control the casting liquid to be extruded from the spinning head at a constant rate and in a fixed quantity, and the core liquid extrusion pump controller (1022) is used to control the core liquid to be extruded from the spinning head at a constant rate and in a fixed quantity.

3. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 2, characterized in that: The spinning head (104) comprises a spinning head casting liquid inlet interface (1041) and a spinning head core liquid inlet interface (1042); the casting liquid extrusion outlet of the casting liquid extrusion pump (101) is connected to the spinning head casting liquid inlet interface (1041); the core liquid extrusion outlet of the core liquid extrusion pump (102) is connected to the spinning head core liquid inlet interface (1042).

4. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: The extrusion molding unit further comprises a lifting mechanism (105), the lifting mechanism (105) comprising: a screw (1051), a spinning head clamping rod (1052), a pulling rotation motor (1053) and a limit switch (1054); the spinning head clamping rod (1052) clamps the spinning head (104); the pulling rotation motor (1053) is transmission-connected to the screw (1051) for driving the screw (1051) to rotate; the spinning head clamping rod (1052) is threadedly connected to the screw (1051); while the pulling rotation motor (1053) drives the screw (1051) to rotate, the spinning head clamping rod (1052) performs lifting and lowering motion along the axial direction of the screw (1051).

5. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: The outside of the spinning chamber (201) is provided with a micro refrigeration compressor (2011), an evaporator (2012), a condenser (2013) and an air-moving motor (2014) which are connected in sequence, and the outlets of the micro refrigeration compressors (2011) are connected to the spinning chamber (201) for controlling the temperature and humidity inside the spinning chamber (201).

6. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: A baffle (2017) having a telescopic hole is arranged at the lower part of the spinning chamber (201), and the telescopic hole of the baffle (2017) and the extrusion hole of the spinning head (104) are arranged on the same straight line.

7. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: A first pumping motor (2021) is installed outside the condensation tank (202), and an outlet of the first pumping motor (2021) is connected to an inlet at the bottom of the condensation tank (202); A first positioning roller (2022), a condensation groove heating tube (2023) and a condensation groove temperature sensor (2024) are arranged inside the condensation groove (202); the condensation groove heating tube (2023) is arranged at the bottom of the condensation groove (202); and the condensation groove temperature sensor (2024) is arranged on an inner wall of one side of the condensation groove (202); a second positioning roller (2025) is arranged at the upper part of the tail end of the condensation groove (202); The first positioning roller (2022) and the second positioning roller (2025) are cooperatively connected to the wire collection and cleaning unit (301).

8. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 1, characterized in that: A third positioning roller (3011) and a wire guide (3012) are arranged on the upper part of the wire collecting and cleaning unit (301), and the third positioning roller (3011) and the wire guide (3012) are connected in cooperation with the second positioning roller (2025); a wire collecting roller (3013) having a motor is arranged inside the wire collecting and cleaning unit (301), and a second water pumping motor (3014) is arranged outside the wire collecting and cleaning unit (301), and the wire collecting roller (3013) is connected in cooperation with the wire guide (3012); the outlet of the second water pumping motor (3014) is connected to the bottom inlet of the wire collecting and cleaning unit (301).

9. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 8, characterized in that: It also includes a controller, and the wire guide machine (3012) includes a wire guide screw. The controller is electrically connected to the wire guide screw and is used to control the movement of the wire guide screw to adjust the wire collection position of the hollow fiber membrane.

10. The hollow fiber membrane substrate preparation device for oil-gas separation according to claim 4, characterized in that: The device also includes a controller, which is electrically connected to the pulling force rotation motor (1053) and the limit switch (1054) respectively, and is used to control the spinning head clamping rod (1052) in the lifting mechanism to move to a preset position.

11. A process for preparing a hollow fiber membrane substrate for oil-gas separation, based on a hollow fiber membrane substrate preparation device for oil-gas separation according to any one of claims 1 to 10, characterized in that: The following steps are involved: Under a preset temperature environment, the casting liquid and the core liquid are subjected to defoaming treatment for a preset time; The casting liquid and the core liquid are squeezed and water-gas induced phase separation is performed simultaneously to obtain a primary hollow fiber membrane; Inducing phase separation in a non-solvent environment to form a hollow fiber membrane; Clean the hollow fiber membrane.

12. The process for preparing a hollow fiber membrane substrate for oil-gas separation according to claim 11, characterized in that: The casting solution is any one of a polyamide-imide / N-methylpyrrolidone solution, a polyvinylidene fluoride / N-methylpyrrolidone solution, a polyamide-imide / dimethyl sulfoxide solution, a polyvinylidene fluoride / dimethyl sulfoxide solution, a polysulfone / N-methylpyrrolidone solution, and a polysulfone / dimethyl sulfoxide solution; The concentration of the casting solution is 15-30wt%.

13. The process for preparing a hollow fiber membrane substrate for oil-gas separation according to claim 11, characterized in that: The core liquid is one or more of N-methylpyrrolidone, dimethylformamide, dimethylacetamide or dimethyl sulfoxide; The core liquid is diluted with deionized water, and the mass percentage of the deionized water is 5-35wt%.

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