CN110681269A - Two-stage coating heterogeneous synchronous composite membrane preparation technology and device - Google Patents

Two-stage coating heterogeneous synchronous composite membrane preparation technology and device Download PDF

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Publication number
CN110681269A
CN110681269A CN201911141198.4A CN201911141198A CN110681269A CN 110681269 A CN110681269 A CN 110681269A CN 201911141198 A CN201911141198 A CN 201911141198A CN 110681269 A CN110681269 A CN 110681269A
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stage coating
membrane
synchronous composite
preparation technology
composite membrane
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CN201911141198.4A
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CN110681269B (en
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廖建
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Ningbo Jian Rong Technology Co Ltd
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Ningbo Jian Rong Technology Co Ltd
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/12Composite membranes; Ultra-thin membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D67/00Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
    • B01D67/0002Organic membrane manufacture
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D69/00Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
    • B01D69/08Hollow fibre membranes

Abstract

The invention discloses a preparation technology of a two-stage coating heterogeneous synchronous composite membrane, which comprises the steps of firstly dissolving a high molecular material and an additive material in a solvent or heating, melting and stirring to form a membrane casting solution, wherein the solvent is a good solvent of the high molecular material, and then extruding the membrane casting solution through a specially designed two-stage coating spinneret plate as a membrane forming channel, wherein the two-stage coating spinneret plate comprises a plurality of filament outlet holes, the preparation technology and the device of the two-stage coating heterogeneous synchronous composite membrane are different from the prior art, the bonding force of a produced hollow fiber membrane is improved, the strength is increased, the water yield is higher while the filtering precision is high, meanwhile, the quality inspection process of the finished product membrane can be simplified through the arranged quality inspection device, the complex processes are effectively reduced, the quality inspection efficiency in the production process of the finished product membrane is effectively improved, and the production and processing efficiency of the hollow fiber membrane is effectively improved, effectively reducing the production cost.

Description

Two-stage coating heterogeneous synchronous composite membrane preparation technology and device
Technical Field
The invention relates to the technical field of hollow fiber membrane preparation, in particular to a preparation technology and a device of a two-stage coating heterogeneous synchronous composite membrane.
Background
Along with the increasingly outstanding environmental problems in recent years, the water resource problem is paid more and more attention, the membrane technology is widely applied to the field of water treatment due to the characteristics of high treatment efficiency, small occupied area, long service life and the like, and particularly, the membrane technology is used for replacing a traditional secondary sedimentation tank to stabilize water outlet and ensure higher sludge concentration at the same time.
However, the conventional spinneret plates for production generally can only realize single-layer coating or interval multi-layer coating, and the spinneret plates have the following problems: (1) the improvement effect on the product performance is small; (2) the coating is carried out at intervals and in multiple layers, so that the preparation process is complicated; (3) the production cost is high, and the single-layer or two-layer composite hollow fiber membrane prepared correspondingly has the following problems: (1) the performance of the film product is single, and the quality is not improved well; (2) the coating is carried out by adopting multiple layers at intervals, so that the adhesion among the layers is poor and the layers are easy to peel; (3) the production process is complex, the efficiency is low, meanwhile, when the quality inspection is carried out in the prior art, the filtration performance detection and the tensile strength performance detection need to be carried out on the membrane component respectively, and when the filtration performance detection and the tensile strength detection are carried out respectively, the membrane component needs to be disassembled and assembled for many times, so that the inconvenience is very high, the detection process is complicated, the quality inspection efficiency in the normal production process is influenced, and further the production and processing efficiency of finished products is influenced.
Disclosure of Invention
The invention aims to provide a two-stage coating heterogeneous synchronous composite membrane preparation technology and a two-stage coating heterogeneous synchronous composite membrane preparation device which have better performance and are convenient to prepare, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a two-stage coating heterogeneous synchronous composite membrane preparing technique includes dissolving high-molecular material and additive material in solvent or heating, melting and stirring to form membrane-casting liquid, using the said solvent as good solvent of the high-molecular material, extruding the membrane-casting liquid through specially designed two-stage coating spinneret plate as membrane-forming channel, contacting with solidification solution or cooling to generate phase inversion, sampling and quality testing the converted product, testing the quality of the product by supporting base, tensile testing machine, weighing mechanism, filtering mechanism, quantitative water tank and conducting mechanism, testing the quality of the product, completing two-stage coating heterogeneous synchronous composite hollow fiber membrane preparation, so that the bonding force of the hollow fiber membrane is improved, the strength is increased, and the filtering precision is high, the water yield is also bigger, simultaneously, through the quality inspection device who sets up, can make finished product membrane quality testing process become simple, has effectively reduced numerous and diverse process to effectively improve the quality testing efficiency in the finished product membrane production process, and then effectively improved the production machining efficiency of hollow fiber membrane, effectively reduced manufacturing cost.
Preferably, the good solvent for the high polymer includes at least one of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, dimethylsulfoxide, acetone, tetrahydrofuran, and triethyl phosphate.
Preferably, the polymer material is polyether sulfone, polyethylene, polypropylene, polytetrafluoroethylene, polyacrylonitrile, polyvinyl chloride, polyimide, polyvinylidene fluoride or the like.
Preferably, the additive material is at least one of absolute ethyl alcohol, polyethylene glycol, lithium nitrate and polyvinylpyrrolidone.
Preferably, the dissolving temperature of the high polymer material and the additive material is 30-200 ℃, and the mass ratio of the high polymer material to the additive is 5-2.
Preferably, the components in the coagulation solution comprise at least one of N-methylpyrrolidone, water, ethanol, glycerol, heptane and pentane, and the temperature of the coagulation bath is maintained at 10-100 ℃, in particular 30-80 ℃.
Preferably, the bore fluid temperature is 20-90 ℃.
Preferably, the two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in a solution at the temperature of 20-60 ℃ for 20-50 hours, and meanwhile, the two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in mixed glycerol water with the volume ratio of 0.2-2 for 20-40 hours for hole protection treatment.
Preferably, a synchronous complex film preparation facilities of two-stage coating heterogeneous, tensile testing machine passes through the support mounting and supports base one end top, weighing machine sets up and is supporting the base top, filtering mechanism sets up at the weighing machine top, the ration water tank is located the filtering mechanism top, conduction mechanism is located between filtering mechanism and the ration water tank, just the ration water tank is through the fixed intercommunication of conduction mechanism and filtering mechanism.
Compared with the prior art, the invention has the beneficial effects that:
compared with the prior art, the invention has the advantages that the bonding force of the produced hollow fiber membrane is improved, the strength is increased, the water yield is higher while the filtration precision is high, meanwhile, the quality inspection process of the finished membrane is simplified through the arranged quality inspection device, and the complicated processes are effectively reduced, so that the quality inspection efficiency in the production process of the finished membrane is effectively improved, the production and processing efficiency of the hollow fiber membrane is effectively improved, and the production cost is effectively reduced.
Drawings
FIG. 1 is a schematic view of the overall structure of the present invention;
FIG. 2 is a schematic view of a partial side plan view of the present invention;
FIG. 3 is a partial perspective view of FIG. 2 according to the present invention;
FIG. 4 is a partial schematic view of FIG. 3 according to the present invention;
FIG. 5 is a schematic view of a filter membrane fixing member according to the present invention;
FIG. 6 is a schematic view of a filter cartridge assembly according to the present invention;
FIG. 7 is a schematic view of an auxiliary connecting cylinder according to the present invention;
FIG. 8 is a schematic view of a portion of the structure of FIG. 7 in accordance with the present invention;
FIG. 9 is a side, partially cross-sectional, plan view of the present invention, as illustrated in FIG. 8;
fig. 10 is a schematic structural diagram of a conduction mechanism according to the present invention.
In the figure: 1-a support base; 2-a tensile testing machine; 3-a weighing mechanism; 4-a filtering mechanism; 5-a quantitative water tank; 6-conducting mechanism; 7-weighing support plate; 8-a weighing sensor; 9-orienting the telescopic rod; 10-a filter cartridge element; 11-auxiliary connecting cylinder; 12-a directional slide rail; 13-a directional slider; 14-filter membrane fixing means; 15-inner cylinder; 16-an outer barrel; 17-water inlet through holes; 18-mounting a collar; 19-stretching the fixed seat; 20-a fixed collar; 21-conducting collar; 22-a conduit; 23-Water inlet manifold.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-10, the present invention provides a technical solution: a two-stage coating heterogeneous synchronous composite membrane preparation technology comprises the steps of firstly dissolving a high polymer material and an additive material in a solvent or heating, melting and stirring to form a membrane casting solution, wherein the solvent is a good solvent of the high polymer material, then extruding the membrane casting solution through a specially designed two-stage coating spinneret plate serving as a membrane forming channel, wherein the two-stage coating spinneret plate comprises a plurality of filament outlet holes, contacting or cooling with a solidification solution after extrusion to generate phase inversion, sampling and quality inspection are carried out on an inverted finished product, the quality inspection of the finished product is mainly realized through a supporting base 1, a tensile testing machine 2, a weighing mechanism 3, a filtering mechanism 4, a quantitative water tank 5 and a conducting mechanism 6, and after the quality inspection is carried out on the finished product, the preparation of the two-stage coating heterogeneous synchronous composite hollow fiber membrane is completed.
The good solvent of the high polymer comprises at least one of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, dimethyl sulfoxide, acetone, tetrahydrofuran and triethyl phosphate.
The high polymer material is polyether sulfone, polyethylene, polypropylene, polytetrafluoroethylene, polyacrylonitrile, polyvinyl chloride, polyimide or polyvinylidene fluoride and the like.
The additive material is at least one of absolute ethyl alcohol, polyethylene glycol, lithium nitrate and polyvinylpyrrolidone.
The dissolving temperature of the high polymer material and the additive material is 30-200 ℃, and the mass ratio of the high polymer material to the additive is 5-2.
The components in the coagulation solution comprise at least one of N-methylpyrrolidone, water, ethanol, glycerol, heptane and pentane, and the temperature of the coagulation bath is maintained at 10-100 deg.C, especially 30-80 deg.C.
The temperature of the core liquid is 20-90 ℃.
The two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in a solution at the temperature of 20-60 ℃ for 20-50 hours, and meanwhile, the two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in mixed glycerol water with the volume ratio of 0.2-2 for 20-40 hours for hole protection treatment.
A two-stage coating heterogeneous synchronous composite membrane preparation device, a tensile testing machine 2 is arranged at the top of one end of a supporting base 1 through a support, a weighing mechanism 3 is arranged at the top of the supporting base 1, a filtering mechanism 4 is arranged at the top of the weighing mechanism 3, a quantitative water tank 5 is arranged above the filtering mechanism 4, a conducting mechanism 6 is arranged between the filtering mechanism 4 and the quantitative water tank 5, the quantitative water tank 5 is fixedly communicated with the filtering mechanism 4 through the conducting mechanism 6, the tensile testing machine 2 is a device in the prior art, preferably an ATH-1000 model, and is not repeated, when in use, a membrane component is arranged in the filtering mechanism 4, is weighed through the weighing mechanism 3, then a fixed amount of fixed mixed liquid is continuously introduced through the quantitative water tank 5, and after the mixed liquid is continuously filtered, the mixed liquid is weighed through the weighing mechanism 3, so that the weight of the filtered impurities can be weighed, thereby obtain the filtration performance of membrane module, then can carry out tensile strength test through setting up the membrane module in tensile test 2 tensile test filter mechanism 4 to make the quality testing in-process can effectively reduce the process, make things convenient for the quality testing, thereby provide its production efficiency.
The weighing mechanism 3 comprises a weighing support plate 7, a weighing sensor 8 is installed at the top of the support base 1, and the weighing support plate 7 is installed at the top of the weighing sensor 8 and used for guaranteeing real-time weighing.
The weighing sensor 8 both sides all are provided with directional telescopic link 9, directional telescopic link 9 both ends respectively with support base 1 and the extension board 7 fixed connection of weighing for improve the stability of extension board 7 in the use of weighing through directional telescopic link 9, guarantee that the device uses stably.
The filtering mechanism 4 comprises a filtering cylinder part 10, the filtering cylinder part 10 is arranged on the top of a weighing support plate 7 through a support, an auxiliary connecting cylinder 11 is fixed on the outer side of the filtering cylinder part 10, a conducting mechanism 6 is arranged on the outer side of the auxiliary connecting cylinder 11, when the filtering mechanism is used, water is continuously supplied into the filtering cylinder part 10 through the auxiliary connecting cylinder 11, so that the detection and comparison of the filtering performance of the filtering cylinder part are facilitated, directional slide rails 12 are arranged at two ends of the top of the weighing support plate 7, the directional slide rails 12 are fixed with the weighing support plate 7 through supports, directional slide blocks 13 are arranged in the directional slide rails 12, filter membrane fixing parts 14 are additionally arranged at two ends of the filtering cylinder part 10, when in quality inspection, a membrane component is put into the filtering cylinder part 10, effective sealing installation of the membrane component is ensured through the filter membrane fixing parts 14, the filter membrane fixing parts 14 and the filtering cylinder part 10 are detachably connected through clamping or bolts and the, therefore, the tensile detection after the detection of the filtering performance is facilitated, when the filter membrane fixing part is stretched, after the filter membrane fixing part 14 and the filter membrane fixing part 10 are disassembled, the tensile strength of the membrane assembly can be directly detected through the tensile testing machine 2 after the tensile testing machine 2 and the filter membrane fixing part 14 are fixedly clamped, the convenience and the practicability are realized, the membrane assembly is prevented from being disassembled and assembled for many times, and the efficiency of detection production is effectively improved.
The filter cylinder part 10 comprises an inner cylinder 15 and an outer cylinder 16, the outer cylinder 16 is sleeved outside the inner cylinder 15, the outer cylinder 16 and the inner cylinder 15 are both provided with water inlet through holes 17 which penetrate through and are communicated, the water inlet through holes 17 comprise a plurality of slotted holes, and the slotted holes are preferably circular hole structures but are not limited.
The filter membrane fixing part 14 comprises an installation lantern ring 18, the installation lantern ring 18 is detachably connected with an outer barrel 16, so that the membrane assembly can be conveniently disassembled in the filter cartridge 10, a stretching fixing seat 19 is fixed to the top of the installation lantern ring 18, the stretching fixing seat 19 is used for being matched with a stretching testing machine 2 to be used, the stretching convenience is guaranteed, a fixing lantern ring 20 is arranged inside the installation lantern ring 18, the fixing lantern ring 20 and the installation lantern ring 18 are detachably connected through threads or bolts, and therefore the membrane assembly and the installation lantern ring 18 can be conveniently disassembled.
Conduction mechanism 6 is including conducting through the lantern ring 21, it is the cavity ring structure to switch on the lantern ring 21, supplementary even 11 lateral walls of a section of thick bamboo run through and be fixed with a plurality of conduction pipes 22, it is located supplementary even 11 outsides of a section of thick bamboo to switch on the lantern ring 21, and switches on lantern ring 21 and a plurality of conduction pipes 22 and all fix the intercommunication, it is fixed with into water branch pipe 23 to run through in addition at lantern ring 21 top to switch on the lantern ring, quantitative water tank 5 is located and switches on lantern ring 21 top, and quantitative water tank 5 and the fixed intercommunication of branch pipe 23 of intaking for cooperation quantitative water tank 5 carries out continuous quantitative water-passing to filter mechanism 4.
It is provided with a plurality ofly, a plurality of to switch on lantern ring 21 equidistance switch on the lantern ring 21 inboard all through switch on pipe 22 with supplementary even a section of thick bamboo 11 fixed intercommunication, and a plurality of switch on lantern ring 21 top all through the fixed intercommunication of branch pipe 23 and quantitative water tank 5 of intaking for accelerate the injection efficiency of mixing liquid in the quantitative water tank 5, thereby effectively improve the efficiency that quality testing in-process filtering quality detected, in order to guarantee to improve the efficiency of finished product membrane production and processing.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (9)

1. A two-stage coating heterogeneous synchronous composite membrane preparation technology comprises the steps of firstly dissolving a high polymer material and an additive material in a solvent or heating, melting and stirring to form a membrane casting solution, wherein the solvent is a good solvent of the high polymer material, then extruding the membrane casting solution through a specially designed two-stage coating spinneret plate serving as a membrane forming channel, wherein the two-stage coating spinneret plate comprises a plurality of filament outlet holes, the two-stage coating spinneret plate is contacted with a solidification solution or cooled to perform phase inversion after being extruded, sampling quality inspection is performed on a converted finished product, the quality inspection of the finished product is mainly realized through a supporting base (1), a tensile testing machine (2), a weighing mechanism (3), a filtering mechanism (4), a quantitative water tank (5) and a conducting mechanism (6), and after the quality inspection is performed on the finished product, the preparation of the two-stage coating heterogeneous synchronous composite.
2. The preparation technology of a two-stage coating heterogeneous synchronous composite membrane according to claim 1, characterized in that: the good solvent of the high polymer comprises at least one of N, N-dimethylformamide, N-dimethylacetamide, N-methylpyrrolidone, dimethyl sulfoxide, acetone, tetrahydrofuran and triethyl phosphate.
3. The preparation technology of a two-stage coating heterogeneous synchronous composite membrane according to claim 2, characterized in that: the high polymer material is polyether sulfone, polyethylene, polypropylene, polytetrafluoroethylene, polyacrylonitrile, polyvinyl chloride, polyimide or polyvinylidene fluoride and the like.
4. A two-stage coating heterogeneous synchronous composite membrane preparation technology according to claim 3, characterized in that: the additive material is at least one of absolute ethyl alcohol, polyethylene glycol, lithium nitrate and polyvinylpyrrolidone.
5. The technology for preparing a two-stage coating heterogeneous synchronous composite membrane according to claim 4, characterized in that: the dissolving temperature of the high polymer material and the additive material is 30-200 ℃, and the mass ratio of the high polymer material to the additive is 5-2.
6. The two-stage coating heterogeneous synchronous composite membrane preparation technology according to claim 5, characterized in that: the components in the coagulation solution comprise at least one of N-methylpyrrolidone, water, ethanol, glycerol, heptane and pentane, and the temperature of the coagulation bath is maintained at 10-100 deg.C, especially 30-80 deg.C.
7. The two-stage coating heterogeneous synchronous composite membrane preparation technology according to claim 6, characterized in that: the temperature of the core liquid is 20-90 ℃.
8. The two-stage coating heterogeneous synchronous composite membrane preparation technology according to claim 7, characterized in that: the two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in a solution at the temperature of 20-60 ℃ for 20-50 hours, and meanwhile, the two-stage coating heterogeneous synchronous composite hollow fiber membrane is soaked in mixed glycerol water with the volume ratio of 0.2-2 for 20-40 hours for hole protection treatment.
9. The preparation device of the two-stage coating heterogeneous synchronous composite membrane according to claim 8, wherein the tensile testing machine (2) is mounted on the top of one end of the supporting base (1) through a bracket, the weighing mechanism (3) is arranged on the top of the supporting base (1), the filtering mechanism (4) is arranged on the top of the weighing mechanism (3), the quantitative water tank (5) is positioned above the filtering mechanism (4), the conducting mechanism (6) is positioned between the filtering mechanism (4) and the quantitative water tank (5), and the quantitative water tank (5) is fixedly communicated with the filtering mechanism (4) through the conducting mechanism (6).
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