CN108452691B - Interfacial polymerization reaction device, and device and method for preparing hollow fiber composite nanofiltration membrane - Google Patents
Interfacial polymerization reaction device, and device and method for preparing hollow fiber composite nanofiltration membrane Download PDFInfo
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- CN108452691B CN108452691B CN201810172608.0A CN201810172608A CN108452691B CN 108452691 B CN108452691 B CN 108452691B CN 201810172608 A CN201810172608 A CN 201810172608A CN 108452691 B CN108452691 B CN 108452691B
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- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
- B01D69/1251—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction by interfacial polymerisation
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Abstract
An interfacial polymerization reaction device, a hollow fiber composite nanofiltration membrane preparation device and a method. The coating assembly comprises a first tank body used for filling a water phase monomer and a second tank body used for filling an oil phase monomer, wherein the first tank body comprises a body, a first communicating part and a second communicating part, the first communicating part is communicated with the body, and the opening of the first communicating part faces upwards. The guide assembly comprises a first guide piece and a second guide piece, the first guide piece is used for guiding a product to be processed into the first groove body from the first communicating part, and the second guide piece is used for guiding the product to be processed into the second groove body from the second communicating part, so that the water phase monomer and the oil phase monomer coated on the product are subjected to interfacial polymerization reaction on the surface of the product to form the composite film. The drying component is arranged between the second communicating part and the second groove body. The device and the method can lead products such as the hollow fiber composite nanofiltration membrane and the like to realize large-scale continuous high-efficiency production in industry.
Description
The technical field of,
The invention relates to the technical field of separation membranes, in particular to an interfacial polymerization reaction device, a preparation device and a preparation method of a hollow fiber composite nanofiltration membrane.
Background
The membrane separation technology uses pressure as a driving force to selectively separate the mixed liquid through the pore size and the surface affinity of the membrane. The composite nanofiltration membrane prepared by the interfacial polymerization method has higher permeation flux and salt rejection rate. In terms of current research reports and practical application, the interfacial polymerization method has a very important position in the basic research and commercialization fields of nanofiltration membranes. The nanofiltration membrane is prepared by an interface polymerization method, and the required composite nanofiltration membrane with excellent mechanical strength, pressure resistance, different selectivity and different permeability can be prepared by independently controlling the structure and the performance of the supporting layer or the compact composite layer.
The composite nanofiltration membrane product comprises a flat membrane component, a hollow fiber membrane component and the like. However, most of the composite nanofiltration membranes on the market are flat membrane components, and hollow fiber membrane components are rarely available. The hollow fiber composite nanofiltration membrane used in the hollow fiber membrane component is generally prepared by adopting interfacial polymerization reaction, and is prepared by soaking and coating in an aqueous phase monomer, taking out and then soaking and coating in an oil phase monomer, so that the industrial large-scale continuous production is difficult. Secondly, the hollow fiber composite nanofiltration membrane has long soaking time for coating the aqueous phase monomer in the interfacial polymerization reaction, which results in lower production efficiency. However, the hollow fiber membrane module has the advantages of more flexible application, high membrane filament loading density, simple raw water pretreatment, low operation and maintenance cost, wider application range and the like, so that an interfacial polymerization reaction device, a hollow fiber composite nanofiltration membrane preparation device and a method which can realize large-scale continuous production in industry are urgently needed to be provided.
Disclosure of Invention
Accordingly, it is necessary to provide an interfacial polymerization reaction apparatus, a hollow fiber composite nanofiltration membrane preparation apparatus and a method, which can industrially realize large-scale continuous and efficient production.
An interfacial polymerization reaction apparatus, comprising:
the coating assembly comprises a first tank body used for filling water phase monomers and a second tank body used for filling oil phase monomers, wherein the first tank body comprises a body, a first communicating part and a second communicating part, the first communicating part and the second communicating part are respectively communicated with the body, and the opening of the first communicating part and the opening of the second communicating part are arranged upwards;
the guide assembly comprises a first guide piece and a second guide piece, the first guide piece is used for guiding a product to be processed into the body of the first groove body from the first communicating part, and the second guide piece is used for guiding the product to be processed coated with the water-phase monomer in the body of the first groove body into the second groove body from the second communicating part so that the water-phase monomer and the oil-phase monomer coated on the product are subjected to interfacial polymerization reaction on the surface of the product to form a composite membrane; and
and the drying assembly is arranged between the second communicating part and the second groove body and used for drying the product to be processed coated with the water phase monomer.
The interfacial polymerization reaction device can be applied to the surface of products such as hollow fiber ultrafiltration support membranes and the like to generate interfacial polymerization reaction to form composite membranes, and then the hollow fiber composite nanofiltration membranes are prepared. Therefore, the products such as the hollow fiber composite nanofiltration membrane and the like which need to be produced by adopting the interfacial polymerization reaction can be industrially produced in a large-scale continuous way, the production efficiency is improved, and in addition, the performance stability of the products such as the hollow fiber composite nanofiltration membrane and the like is also improved.
In one embodiment, the device further comprises a first heating assembly for heating the first tank body and/or a second heating assembly for heating the second tank body.
In one embodiment, the coating assembly further comprises a first temperature control element for regulating and controlling the temperature of the water phase monomer in the first tank body and/or a second temperature control element for regulating and controlling the temperature of the oil phase monomer in the second tank body.
In one embodiment, the coating assembly further comprises a first pressure monitoring piece for monitoring the hydraulic pressure of the liquid level of the product to be processed in the body of the first tank body and/or a second pressure monitoring piece for monitoring the hydraulic pressure of the liquid level of the product to be processed in the second tank body.
In one embodiment, the first groove body is of a U-shaped structure.
In one embodiment, the first groove body is formed by connecting a plurality of sections of pipelines with openings at two ends through flanges.
In one embodiment, the drying assembly comprises a power source and an air drying pipe, the power source is used for providing compressed air for the air drying pipe, the air drying pipe is arranged between the second communicating part and the second groove body, the pipe wall of the air drying pipe is of a hollow structure, the pipe wall is provided with a ventilation inner cavity communicated with the power source, and an air outlet hole is formed in the inner surface of the pipe wall so as to air-dry a product to be processed which passes through the pipe hole of the air drying pipe.
The preparation device of the hollow fiber composite nanofiltration membrane comprises a heat treatment device and the interfacial polymerization reaction device, wherein the interfacial polymerization reaction device is used for carrying out interfacial polymerization reaction on the surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer, and the heat treatment device is used for carrying out heat treatment on the hollow fiber ultrafiltration support membrane formed with the composite membrane separation layer to prepare the hollow fiber composite nanofiltration membrane.
A preparation method of a hollow fiber composite nanofiltration membrane uses the preparation device of the hollow fiber composite nanofiltration membrane, and the preparation method comprises the following steps:
sequentially enabling the hollow fiber ultrafiltration support membrane to pass through the first communicating part, the body, the second communicating part, the drying component and the second groove body through the first guiding part and the second guiding part, coating a water phase monomer in the first groove body, drying through the drying component, coating an oil phase monomer in the second groove body, and enabling the water phase monomer and the oil phase monomer to perform interfacial polymerization reaction on the surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer; and then carrying out heat treatment on the heat treatment device to obtain the hollow fiber composite nanofiltration membrane.
In one embodiment, the hollow fiber ultrafiltration support membrane is made of polysulfone, polyethersulfone, polyethylene, polypropylene, polyvinyl chloride, polyimide, polyacrylonitrile, polyvinylidene fluoride, polytetrafluoroethylene or polyester;
the water phase monomer is an aqueous solution of at least one of piperazine, triaminobenzene, p-aminobenzene, m-aminobenzene, polyethylene glycol sulfate, polyethylene glycol phosphate, quaternized polyethylene glycol and polyethylene glycol amphoteric polyelectrolyte; the mass fraction of the aqueous solution is 0.5-5%;
the oil phase monomer is a mixed solution of organic solvent and at least one of trimesoyl chloride, terephthaloyl chloride, isophthaloyl chloride, diisocyanate, epichlorohydrin, diglycidyl ether and glycerol glycidyl ether; the organic solvent is at least one of n-hexane and toluene;
the liquid level of the first tank body is 0.5-5 m, the coating time of the water phase monomer is 0.5-5 minutes, and the coating time of the oil phase monomer is 10-60 seconds.
Drawings
FIG. 1 is a schematic diagram of an interfacial polymerization apparatus according to an embodiment.
Detailed Description
In order that the invention may be more fully understood, a more particular description of the invention will now be rendered by reference to specific embodiments thereof that are illustrated in the appended drawings. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Referring to fig. 1, an interfacial polymerization apparatus 10 according to an embodiment includes a coating unit, a guide unit, and a drying unit 14.
The coating assembly comprises a first tank 11 for filling the water phase monomer and a second tank 12 for filling the oil phase monomer. The first tank 11 includes a main body 111, a first communicating portion 112 and a second communicating portion 113, and the first communicating portion 112 and the second communicating portion 113 are respectively communicated with the main body 111 and have upward openings.
The guide assembly includes a first guide 131 and a second guide 132. The first guide 131 is used to guide the product to be processed from the first communicating portion 112 into the body 111 of the first tank body 11. The second guiding member 132 is used for guiding the product to be processed coated with the aqueous phase monomer in the body 111 of the first tank body 11 into the second tank body 12 from the second communicating part 113, so that the aqueous phase monomer coated on the product and the oil phase monomer are subjected to interfacial polymerization reaction on the surface of the product to form a composite film.
The drying component 14 is arranged between the second communicating part 113 and the second groove body 12 and is used for drying the product to be processed coated with the water phase monomer, removing redundant water on the surface of the product, and controlling the drying degree of the product to be processed before the film silk enters the oil phase monomer.
When the interfacial polymerization reaction device 10 works, the first tank body 11 and the second tank body 12 are respectively filled with the water phase monomer and the oil phase monomer, and other products to be processed, such as the hollow fiber ultrafiltration support membrane, are arranged on the first guide member 131 and the second guide member 132 and sequentially pass through the first communicating part 112, the body 111, the second communicating part 113, the drying component 14 and the second tank body 12, so that the water phase monomer and the oil phase monomer are subjected to interfacial polymerization reaction on the surfaces of the products, such as the hollow fiber ultrafiltration support membrane, to form the composite membrane. The water phase monomer and the oil phase monomer of the interfacial polymerization reaction have high activity, and once the monomers are contacted with each other, a net-shaped ultrathin compact surface layer is quickly formed on the surface of a product, namely the composite film. And finally, obtaining the hollow fiber composite nanofiltration membrane through heat treatment.
Above-mentioned interfacial polymerization reaction unit 10 adopts direction subassembly with aqueous phase monomer coating and oil phase monomer coating serialization, adopts drying assembly 14 to detach the excessive moisture in the product surface of treating that coats and has coated the aqueous phase monomer, has overcome the problem that silk membraniform products such as hollow fiber ultrafiltration supporting membrane can't brush unnecessary liquid through the brush like flat supporting layer, avoids unnecessary liquid and coating inhomogeneous to lead to the fact the complex film to form "pinhole" defect, and then influences the problem of the infiltration interception performance of hollow fiber composite nanofiltration membrane. Moreover, through the unique design of the first tank body 11, the liquid levels of the first communicating part 112 and the second communicating part 113 can be controlled, so as to control the liquid levels of products such as hollow fiber ultrafiltration support membranes in the body 111 of the first tank body 11, further increase the pressure of the hollow fiber ultrafiltration support membranes in the water phase coating process through higher liquid levels, accelerate the permeation and adsorption rates of products such as water phase monomers and hollow fiber ultrafiltration support membranes, further shorten the soaking time required by water phase coating, further shorten the soaking time required by water phase monomer coating, further reduce the difference between the soaking times required by water phase monomer coating and oil phase monomer coating, further reduce the production time on the basis of continuous production, and improve the production efficiency.
Therefore, the application of the interfacial polymerization reaction device 10 not only enables the products such as the hollow fiber composite nanofiltration membrane and the like which need to be produced by the interfacial polymerization reaction to be industrially produced in a large-scale continuous way, but also improves the production efficiency, and in addition, improves the performance stability of the products such as the hollow fiber composite nanofiltration membrane and the like.
Specifically, in the conventional preparation method, the coating time of the aqueous phase monomer, i.e., the time of the reaction with the aqueous phase monomer, is at least 5-20 minutes, and the coating time of the aqueous phase monomer can be shortened to 0.5-5 minutes by using the interfacial reaction device.
It will be appreciated that the interfacial polymerization apparatus 10 described above may be used for interfacial polymerization of one or more hollow fiber ultrafiltration support membranes while waiting for a process product, and may also be used for surface chemical modification of the membranes. In particular, in order to avoid the mutual influence of a plurality of hollow fiber ultrafiltration support membranes, the guide assembly can be modified appropriately to provide grooves or baffles. The method for preparing the composite membrane by interfacial polymerization has the advantage of adjustable structure of the thickness and the aperture of the compact layer, thereby breaking through the limitation of the trade-off between the water flux and the rejection rate of the separation membrane prepared by the conventional process, and simultaneously improving the permeation flux and the rejection rate of the prepared composite membrane.
Further, the interfacial polymerization apparatus 10 further comprises a first heating element (not shown). The first heating assembly is used for heating the first tank body 11. Further, the interfacial polymerization apparatus 10 further comprises a second heating element (not shown). The second heating assembly is used for heating the second tank body 12. The heating temperature of the first heating assembly can thus be set according to the temperature required for aqueous monomer coating. The heating temperature of the second heating assembly may be set according to the temperature required for oil phase monomer coating.
Further, the coating assembly also includes a first temperature control 114. The first temperature control element 114 is used for adjusting and controlling the temperature of the aqueous phase monomer in the first tank body 11. Further, the coating assembly further comprises a second temperature control (not shown). The second temperature control element is used for adjusting and controlling the temperature of the oil phase monomer in the second tank body 12.
Further, the coating assembly further comprises a first pressure monitoring member 115. The first pressure monitoring member 115 is used for monitoring the hydraulic pressure of the liquid level of the product to be processed in the body 111 of the first tank 11. Further, the coating assembly further comprises a second pressure monitoring member (not shown). The second pressure monitoring part is used for monitoring the hydraulic pressure of the liquid level of the product to be processed in the second tank body 12. The first pressure monitoring part and the second pressure monitoring part are pressure gauges.
Specifically, the first tank 11 has a U-shaped structure. The first tank body 11 with the U-shaped structure can reduce the usage amount of the water phase monomer. That is, the body 111, the first communicating portion 112 and the second communicating portion 113 of the first tank 11 together form a U-shaped structure. Specifically, the first tank 11 is formed by connecting a plurality of sections of pipes with openings at both ends through flanges. The first tank 11 is thus very flexible in arrangement, and the heights of the first communicating portion 112 and the second communicating portion 113 can also be flexibly arranged as needed. Specifically, the pipe is a steel pipe.
Specifically, the bottom of the body 111 of the first tank 11 is provided with a first drain port (not shown). The bottom of the second tank body 12 is provided with a second liquid outlet (not shown).
Further, the drying assembly 14 includes a power source (not shown) and an air-drying duct (not shown). The power source is used for supplying compressed gas to the air drying pipe, and the air drying pipe is arranged between the second communicating part 113 and the second groove body 12.
Specifically, the power source is an air compressor. Specifically, the pipe wall of the air drying pipe is of a hollow structure and is provided with a ventilation inner cavity used for being communicated with a power source. The pipe wall is communicated with the power source, and the inner surface of the pipe wall is provided with an air outlet hole so as to uniformly air-dry products inside the air drying pipe, and the air drying degree is controllable. More specifically, the number of the air outlet holes may be plural. Specifically, the ventilation inner cavity enables compressed air to form fine air flow in the ventilation inner cavity, so that the compressed air can uniformly flow out from the air outlet through the fine air flow channel, and a product to be processed is uniformly air-dried. More specifically, the air outlet holes are uniformly distributed on the inner surface of the air drying pipe so as to air-dry the product to be processed by 360 degrees.
Specifically, the drying assembly 14 further includes a heating temperature control component, which can perform precise heating temperature control on the gas flowing through.
Specifically, the drying assembly 14 further includes a third pressure monitoring and adjusting member (not shown) disposed on a pipeline connecting the air drying pipe and the power source for adjusting and monitoring the air outlet speed. The third pressure monitoring and adjusting part is a pressure gauge.
More specifically, the interfacial polymerization apparatus 10 further comprises a first support 15 and a second support 16. The first bracket 15 is connected to the first communicating portion 112, the body 111, and the second communicating portion 113 of the first tank 11, respectively, to ensure stability thereof. A second bracket 16 is connected to the second tank 12 for supporting the second tank 12.
Specifically, the first guide 131 is connected to the first bracket 15 and located at the opening of the first communicating portion 112. Specifically, the air drying pipe is connected to the first support 15 and disposed opposite to the opening of the second communicating portion 113. Specifically, the second guide 132 is connected to the first bracket 15 and is located at an opening of the seasoning pipe away from the first communicating portion 112.
Specifically, the first bracket 15 has a rectangular frame structure, the first slot 11 is located in the first bracket 15, and the first communicating portion 112, the body 111, and the second communicating portion 113 are respectively connected to the first bracket 15. Specifically, the second bracket 16 is provided at one side of the first bracket 15. More specifically, the first bracket 15 and the second bracket 16 are located in one plane.
Specifically, the first bracket 15 is further provided with a reinforcing rib. The reinforcing beads are horizontally disposed in parallel with the junction of the first guide 131 and the second guide 132.
More specifically, the first bracket 15 and the second bracket 16 are connected to each other to enhance the overall stability of the interface reaction apparatus.
Specifically, the guiding assembly further comprises a third guiding element 133, and the third guiding element 133 is disposed on the first bracket 15 and is used for providing a buffering section for the product to be processed coming out of the air drying pipe before entering the second groove 12. Specifically, the number of the third guiding elements 133 is plural, the plural third guiding elements 133 are arranged on the first bracket 15 at intervals, and the distance between two adjacent third guiding elements 133 and the first bracket 15 is different, so as to further increase the buffering section.
In particular, each guide is a guide wheel. The surface of each guide member is provided with sponge foam to reduce the abrasion of the surface of the product by the guide member. Specifically, the sponge foam is high-molecular polymer soft sponge foam. More specifically, the sponge foam is made of at least one material selected from polyurethane, polyethylene, phenolic resin, polyether, polyvinyl alcohol and natural latex.
Further, the interfacial polymerization apparatus 10 further includes an unwinding assembly. The unwinding assembly is disposed at an opening of the first communicating portion 112, and is used for unwinding a product to be coated. Specifically, unreel the subassembly and have the unreel wheel, the surface of unreeling the wheel also can be equipped with above-mentioned sponge foam. It is understood that in one embodiment, the first guide 131 can replace the unwind wheel, while serving both unwinding and guiding functions.
Further, the interfacial polymerization reaction device 10 further comprises a winding component 17. The rolling component 17 is arranged on one side of the second tank body 12 and is used for rolling the product after the interfacial polymerization reaction. Specifically, rolling component 17 has the rolling wheel, and the surface of rolling wheel also can be equipped with above-mentioned sponge foam. The take-up reel is attached to the second support 16.
The invention also provides a preparation device of the hollow fiber composite nanofiltration membrane. It comprises a heat treatment device and the interfacial polymerization reaction device 10.
The interfacial polymerization apparatus 10 is used to perform interfacial polymerization on the surface of a hollow fiber ultrafiltration support membrane to form a composite membrane separation layer.
The heat treatment device is used for carrying out heat treatment on the hollow fiber membrane with the composite membrane separation layer so as to further crosslink and polymerize the composite membrane separation layer and further shrink and densify micropores on the surface layer, and the hollow fiber composite nanofiltration membrane is obtained.
Specifically, the heat treatment apparatus is an oven or the like that can perform heat treatment.
The preparation device of the hollow fiber composite nanofiltration membrane can be used for large-scale continuous production of the hollow fiber composite nanofiltration membrane, and has higher production efficiency and product performance stability.
The prepared hollow fiber composite nanofiltration membrane takes a hollow fiber ultrafiltration support membrane as a middle support layer, and a composite membrane separation layer is a compact composite separation layer which is tightly and uniformly combined on the outer surface of the hollow fiber ultrafiltration support membrane.
The invention also provides a preparation method of the hollow fiber composite nanofiltration membrane, and a preparation device using the hollow fiber composite nanofiltration membrane. The preparation method comprises the following steps:
the hollow fiber ultrafiltration support membrane sequentially passes through the first communicating part, the body, the second communicating part, the drying component and the second groove body through the first guiding part and the second guiding part. Coating a water phase monomer in the first tank body by the hollow fiber ultrafiltration support membrane, drying by a drying component, coating an oil phase monomer in the second tank body, and performing interfacial polymerization reaction on the water phase monomer and the oil phase monomer on the surface of the hollow fiber ultrafiltration support membrane to form a composite membrane; and then carrying out heat treatment in a heat treatment device to obtain the hollow fiber composite nanofiltration membrane.
The preparation method of the hollow fiber composite nanofiltration membrane is simple, the cost is low, continuous and efficient production can be realized, and the prepared hollow fiber composite nanofiltration membrane has high performance stability.
Furthermore, the hollow fiber ultrafiltration support membrane is made of polysulfone, polyethersulfone, polyethylene, polypropylene, polyvinyl chloride, polyimide, polyacrylonitrile, polyvinylidene fluoride, polytetrafluoroethylene or polyester.
Specifically, the hollow fiber ultrafiltration membrane support layer can be directly purchased or prepared by a thermally induced phase separation method, a non-solvent induced phase separation method and a thermal stretching method.
Further, the water phase monomer is at least one aqueous solution of piperazine, triaminobenzene, p-aminobenzene, m-aminobenzene, polyethylene glycol sulfate, polyethylene glycol phosphate, quaternized polyethylene glycol and polyethylene glycol amphoteric polyelectrolyte; the mass fraction of the aqueous solution is 0.5-5%.
Further, the oil phase monomer is a mixed solution of at least one of trimesoyl chloride, terephthaloyl chloride, isophthaloyl chloride, diisocyanate, epichlorohydrin, diglycidyl ether and glycerol glycidyl ether and an organic solvent, wherein the organic solvent is at least one of n-hexane and toluene.
In this embodiment, the coating time of the oil phase monomer, that is, the time of the hollow fiber ultrafiltration support membrane coated with the water phase monomer passing through the second tank is 10 to 60 seconds. Therefore, in order to further realize continuous and efficient production, the coating time of the aqueous phase monomer is as close as possible to the coating time. In one embodiment, the liquid level of the first tank body is 0.5-5 m, namely the liquid level of the hollow fiber ultrafiltration support membrane in the body of the first tank body is 0.5-5 m. The time of the hollow fiber ultrafiltration support membrane passing through the water phase monomer in the first tank body can be controlled to be 0.5-5 minutes by controlling the path of the water phase monomer passing through the hollow fiber ultrafiltration support membrane and the transmission speed of the guide component, namely the coating time of the water phase monomer is 0.5-5 minutes. Preferably, the coating time of the aqueous phase monomer can be made to be equivalent to that of the oil phase monomer by adjusting the liquid level and the transfer speed of the guide member.
Specifically, the heat treatment is carried out under the condition of 70-100 ℃ for 10-50 minutes.
The following are specific examples. The following examples were all prepared using the interfacial polymerization apparatus 10 shown in FIG. 1.
Example 1
Preparing the hollow fiber ultrafiltration support membrane. The hollow fiber ultrafiltration support membrane is spun on a hollow fiber spinning machine by using 17 wt% of polyvinylidene fluoride as a main material, 12 wt% of polyethylene glycol 200, 8 wt% of polyethylene glycol 20000 as a pore-forming agent, 63 wt% of dimethylacetamide as a solvent and water as a core solution and an external coagulation bath.
And after the spun hollow fiber ultrafiltration support membrane is cleaned and dried, taking down the hollow fiber ultrafiltration support membrane together with a wire winding wheel and installing the hollow fiber ultrafiltration support membrane on an unwinding wheel of an unwinding assembly of the interface reaction device. One end of the hollow fiber ultrafiltration support membrane is pulled out. After ensuring that the membrane filaments on the equipment run smoothly, adding triaminobenzene water solution with the mass fraction of 2wt percent as a water phase monomer into the first tank body until the liquid level of the hollow fiber ultrafiltration support membrane in the tank body is 3.5 meters. 0.1 wt% of trimesic acid chloride normal hexane solution is added into the second tank body as an oil phase monomer. And starting equipment, adjusting the speed of the wire feeding wheel and the speed of the wire collecting wheel, opening the blow-drying equipment, sequentially passing through the first communicating part, the body, the second communicating part, the drying component and the second groove body through the guide component, and continuously coating the outer surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer. The oil phase monomer was applied for 60 seconds and the water phase monomer was applied for 1 minute.
And after the whole film winding silk is coated, taking down the whole film winding silk and carrying out heat treatment at 85 ℃ for 30 minutes to obtain the hollow fiber composite nanofiltration membrane with the compact composite separation layer.
Example 2
Preparing the hollow fiber ultrafiltration support membrane. The hollow fiber ultrafiltration support membrane is spun on a hollow fiber spinning machine by taking 19 wt% of polyether sulfone as a main material, 10 wt% of polyvinylpyrrolidone and 8 wt% of n-propanol as pore-forming agents, 63 wt% of dimethylacetamide as a solvent and water as core solution and an external coagulation bath.
And after the spun hollow fiber ultrafiltration support membrane is cleaned and dried, taking down the hollow fiber ultrafiltration support membrane together with a wire winding wheel and installing the hollow fiber ultrafiltration support membrane on an unwinding wheel of an unwinding assembly of the interface reaction device. One end of the hollow fiber ultrafiltration support membrane is pulled out. After ensuring that membrane filaments on the equipment run smoothly, adding a quaternized polyethylene glycol aqueous solution with the mass fraction of 1.5 wt% as a water-phase monomer into the first tank body until the liquid level of the hollow fiber ultrafiltration support membrane in the tank body is 2 m. And adding 0.1 wt% of epichlorohydrin normal hexane solution serving as an oil phase monomer into the second tank. And starting equipment, adjusting the speed of the wire feeding wheel and the speed of the wire collecting wheel, opening the blow-drying equipment, sequentially passing through the first communicating part, the body, the second communicating part, the drying component and the second groove body through the guide component, and continuously coating the outer surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer. The oil phase monomer was applied for 60 seconds and the water phase monomer was applied for 1.5 minutes.
And after the whole film winding silk is coated, taking down the whole film winding silk, and carrying out heat treatment at 100 ℃ for 12 minutes to obtain the hollow fiber composite nanofiltration membrane with the compact composite separation layer.
Example 3
The preparation method of example 3 is substantially the same as that of example 1 except that the hollow fiber ultrafiltration support membrane in the body is at a liquid level of 5m, the coating time of the oil phase monomer is 30 seconds, the coating time of the water phase monomer is 0.5 minutes, and the heat treatment conditions are 70 ℃ for 50 minutes.
Comparative example 1
The hollow fiber ultrafiltration support membrane, the aqueous phase monomer, the oil phase monomer and the heat treatment conditions were the same as in example 1.
And (3) placing the hollow fiber ultrafiltration support membrane in the water phase monomer for soaking for 10 minutes, taking out and naturally drying. And (3) placing the hollow fiber ultrafiltration membrane in an oil phase monomer for 60 seconds to carry out interfacial polymerization reaction so as to form a composite membrane separation layer on the outer surface of the hollow fiber ultrafiltration support membrane, taking out the hollow fiber ultrafiltration support membrane, cleaning and drying the hollow fiber ultrafiltration support membrane, and then carrying out heat treatment to obtain the hollow fiber composite nanofiltration membrane.
It is obvious from actual production that the production efficiency of comparative example 1 is lower than that of examples 1 to 3. And the yield of the hollow fiber composite nanofiltration membrane prepared in the comparative example 1 and the examples 1 to 3 is analyzed, the yield of the comparative example 1 is 80%, and the yields of the examples 1 to 3 are all 90%. The coating of comparative example 1 was less uniform and the coating process and coating time were difficult to control precisely, resulting in poor reproducibility thereof.
In addition, qualified hollow fiber composite nanofiltration membranes prepared in the comparative example 1 and the examples 1 to 3 are tested under 0.2MPa for pure water flux and Na with the concentration of 1000ppm2SO4Has a retention rate and a MgCl concentration of 1000ppm2The retention rate of (1), the obtained average value of pure water flux, Na2SO4Average value of rejection and MgCl2The results are shown in the following table. Therefore, the preparation method can also improve the separation efficiency.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. An interfacial polymerization reaction apparatus, comprising:
the coating assembly comprises a first tank body used for filling water phase monomers and a second tank body used for filling oil phase monomers, the first tank body comprises a body, a first communicating part and a second communicating part, the first communicating part and the second communicating part are respectively communicated with the body, the opening of the first communicating part and the opening of the second communicating part are arranged upwards, the first communicating part and the second communicating part and the body form a U-shaped structure together, and the bottom of the second tank body is provided with a liquid discharge port;
the guide assembly comprises a first guide piece and a second guide piece, the first guide piece is used for guiding a product to be processed into the body of the first groove body from the first communicating part, and the second guide piece is used for guiding the product to be processed coated with the water-phase monomer in the body of the first groove body into the second groove body from the second communicating part so that the water-phase monomer and the oil-phase monomer coated on the product are subjected to interfacial polymerization reaction on the surface of the product to form a composite membrane; and
and the drying assembly is arranged between the second communicating part and the second groove body and used for drying the product to be processed coated with the water phase monomer.
2. The interfacial polymerization reaction apparatus of claim 1, further comprising a first heating assembly for heating the first tank and/or a second heating assembly for heating the second tank.
3. The interfacial polymerization reaction device of claim 2, wherein the coating assembly further comprises a first temperature control element for regulating and controlling the temperature of the aqueous phase monomer in the first tank and/or a second temperature control element for regulating and controlling the temperature of the oil phase monomer in the second tank.
4. The interfacial polymerization apparatus of claim 2, wherein the coating assembly further comprises a first pressure monitoring member for monitoring a hydraulic pressure of a liquid level of the product to be processed in the body of the first tank and/or a second pressure monitoring member for monitoring a hydraulic pressure of a liquid level of the product to be processed in the second tank.
5. The interfacial polymerization apparatus of claim 1, wherein the bottom of the body of the first tank is also provided with a drain.
6. The interfacial polymerization apparatus of claim 5, wherein the first tank is formed by connecting a plurality of sections of pipes with openings at both ends via flanges.
7. The interfacial polymerization reaction device according to any one of claims 1 to 6, wherein the drying assembly comprises a power source and an air drying pipe, the power source is used for providing compressed gas for the air drying pipe, the air drying pipe is arranged between the second communicating portion and the second groove body, a pipe wall of the air drying pipe is of a hollow structure, the pipe wall is provided with a ventilation inner cavity used for communicating with the power source, and an air outlet is formed in the inner surface of the pipe wall so as to air-dry a product to be processed which passes through a pipe hole of the air drying pipe.
8. The preparation device of the hollow fiber composite nanofiltration membrane is characterized by comprising a heat treatment device and the interfacial polymerization reaction device as claimed in any one of claims 1 to 7, wherein the interfacial polymerization reaction device is used for performing interfacial polymerization reaction on the surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer, and the heat treatment device is used for performing heat treatment on the hollow fiber membrane with the composite membrane separation layer to prepare the hollow fiber composite nanofiltration membrane.
9. A method for preparing a hollow fiber composite nanofiltration membrane, which is characterized in that the device for preparing the hollow fiber composite nanofiltration membrane as claimed in claim 8 is used, and the method comprises the following steps:
sequentially enabling the hollow fiber ultrafiltration support membrane to pass through the first communicating part, the body, the second communicating part, the drying component and the second groove body through the first guiding part and the second guiding part, coating a water phase monomer in the first groove body, drying through the drying component, coating an oil phase monomer in the second groove body, and enabling the water phase monomer and the oil phase monomer to perform interfacial polymerization reaction on the surface of the hollow fiber ultrafiltration support membrane to form a composite membrane separation layer; and then carrying out heat treatment on the heat treatment device to obtain the hollow fiber composite nanofiltration membrane.
10. The method for preparing the hollow fiber composite nanofiltration membrane according to claim 9, wherein the hollow fiber ultrafiltration support membrane is made of polysulfone, polyethersulfone, polyethylene, polypropylene, polyvinyl chloride, polyimide, polyacrylonitrile, polyvinylidene fluoride, polytetrafluoroethylene or polyester;
the water phase monomer is an aqueous solution of at least one of piperazine, triaminobenzene, p-aminobenzene, m-aminobenzene, polyethylene glycol sulfate, polyethylene glycol phosphate, quaternized polyethylene glycol and polyethylene glycol amphoteric polyelectrolyte; the mass fraction of the aqueous solution is 0.5-5%;
the oil phase monomer is a mixed solution of organic solvent and at least one of trimesoyl chloride, terephthaloyl chloride, isophthaloyl chloride, diisocyanate, epichlorohydrin, diglycidyl ether and glycerol glycidyl ether; the organic solvent is at least one of n-hexane and toluene;
the liquid level of the first tank body is 0.5-5 m, the coating time of the water phase monomer is 0.5-5 minutes, and the coating time of the oil phase monomer is 10-60 seconds.
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| PCT/CN2018/081413 WO2019165664A1 (en) | 2018-03-01 | 2018-03-30 | Interfacial polymerization reaction device, and hollow fiber composite nanofiltration membrane preparation device and method |
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