CN113019152A - High-performance nanofiltration membrane, preparation process and direct drinking water device using high-performance nanofiltration membrane - Google Patents
High-performance nanofiltration membrane, preparation process and direct drinking water device using high-performance nanofiltration membrane Download PDFInfo
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- CN113019152A CN113019152A CN202110224242.9A CN202110224242A CN113019152A CN 113019152 A CN113019152 A CN 113019152A CN 202110224242 A CN202110224242 A CN 202110224242A CN 113019152 A CN113019152 A CN 113019152A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/30—Polyalkenyl halides
- B01D71/32—Polyalkenyl halides containing fluorine atoms
- B01D71/34—Polyvinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
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Abstract
The application relates to the field of nanofiltration membranes, and more particularly relates to a high-performance nanofiltration membrane, a preparation process and a direct drinking water device using the same, wherein the invention provides the high-performance nanofiltration membrane, the high-performance nanofiltration membrane comprises a first support layer microporous channel, a second support layer microporous channel and a third support layer microporous channel, the first support layer microporous channel is close to the outer surface of the high-performance nanofiltration membrane, the third support layer is close to the inner surface of the high-performance nanofiltration membrane, the second support layer microporous channel is located between the third support layer microporous channel and the first support layer microporous channel, the high-performance nanofiltration membrane further comprises an open side and a interception side, and the average pore diameter of the open side and the interception side is 25-250nm1-10nm respectively. The invention has uniform membrane aperture distribution, and can greatly relieve the problems of membrane and ultrafiltration basal membrane peeling generated in the application process of the composite nanofiltration membrane of interfacial polymerization reaction, non-uniform membrane aperture retention solution, easy aperture closing, short storage time and the like.
Description
Technical Field
The application relates to the field of nanofiltration membranes, in particular to a high-performance nanofiltration membrane, a preparation process and a direct drinking water device using the same.
Background
There are some problems with current high performance nanofiltration membranes, such as: the high-performance nanofiltration membrane has the advantages of easy pore diameter closing, short storage time, long process flow, low porosity, short service life, low water yield and high energy consumption. In addition, the preparation process of the high-performance nanofiltration membrane has some problems, such as: the problem that the pore size of the membrane is not uniform due to nonuniform heating temperature of the materials during dissolution exists in the process of the extraction step of the spinning solution. The method comprises the following steps of post-processing and hole-keeping, wherein the problems of non-uniform film hole-keeping liquid, long film hole-keeping time and short film storage time are solved in the post-processing and hole-keeping step, the problem of serious solvent loss caused by poor defoaming time in the vacuum defoaming step is solved, and the problem of non-uniform film hole diameter forming size caused by non-uniform stress tensile strength of the inner side and the outer side of a circular winding roller and a film wire in a close contact manner is solved in the curing step. In addition, the water drinking device using the high-performance nanofiltration membrane is inconvenient to install and place due to the structural design problem, and poor in sealing performance.
Therefore, a need exists for a high-performance nanofiltration membrane, a preparation process and a direct drinking water device using the same, which can solve the above problems.
Disclosure of Invention
The main objective of this application provides an use straight drinking water device of high performance nanofiltration membrane, wherein, straight drinking water device includes a jar body, jar body includes a casing and two rotating member, two the rotating member is rotationally connected in the both ends of casing.
Another object of the present application is to provide a process for preparing a high-performance nanofiltration membrane, wherein the process for preparing a high-performance nanofiltration membrane has the following advantages:
1. in the step of extracting the spinning solution, the forward rotation and reverse rotation stirring speeds of the crusher are combined, so that the problem of nonuniform membrane aperture size caused by nonuniform heating temperature of the materials during dissolution is solved;
2. in the post-processing hole-protecting step, the sound energy of a power ultrasonic frequency source is converted into mechanical vibration by utilizing the ultrasonic principle, the hole-protecting liquid in the groove is radiated to ultrasonic waves through the wall of the hole-protecting groove, and micro bubbles in the liquid in the groove can keep vibrating under the action of the sound waves due to the radiated ultrasonic waves, so that the film hole-protecting liquid is uniform, the film hole-protecting time is shortened, and the storage time of the film is prolonged;
3. in the vacuum defoaming step, the spinning solution is guided to the inner wall of the vacuum defoaming device by the drainage rod and flows into the tank bottom, so that a large amount of bubbles are generated in the vacuum extraction process, the defoaming time is shortened, and the solvent loss is reduced;
4. in the curing step, a positive guide wire, a negative guide wire, a positive guide wire and a negative guide wire are used for positive and negative stretching, so that the problem that the aperture of a tangent point of a single positive guide wire and a membrane wire is not uniform in tensile strength with other parts, the membrane aperture forming forms are different, and the membrane aperture size is not uniform is solved; 5. in the curing step, the polygonal swinging needle type flat plate is used for winding and collecting the film, so that the problem that the forming size of the aperture of the film is not uniform due to uneven stressed tensile strength of the inner side and the outer side of a circular winding roller, which are tightly attached to the film wire, is solved;
6. because internal pressure operation and external pressure backwashing or external pressure backwashing and internal pressure operation are adopted, cross-flow filtration is realized, and the problems of short service life, low water yield and the like are solved;
7. because the parameters of each step are scientifically, reasonably and optimally selected, the prepared high-performance nanofiltration membrane has uniform membrane pore size distribution, and can greatly relieve the problems of peeling of a membrane and an ultrafiltration base membrane, nonuniform material dissolution and heating, long dissolution time, nonuniform membrane pore size retention solution and short pore size easy closing storage time in the application process of the composite nanofiltration membrane for interfacial polymerization reaction.
Another object of the present invention is to provide a high performance nanofiltration membrane, wherein the high performance nanofiltration membrane has a first support layer microporous channel, a second support layer microporous channel, and a third support layer microporous channel, the first support layer microporous channel is close to the outer surface of the high performance nanofiltration membrane, the third support layer is close to the inner surface of the high performance nanofiltration membrane, and the second support layer microporous channel is located between the third support layer microporous channel and the first support layer microporous channel, wherein the high performance nanofiltration membrane further has an open side and a trapped side, and the average pore diameters of the open side and the trapped side are 25-250nm and 1-10nm, respectively.
Another aim at of this application provides a high performance nanofiltration membrane, preparation technology and use its straight drinking water device, wherein, high performance nanofiltration membrane, preparation technology and use its straight drinking water device simple structure, simple operation do not relate to complicated manufacturing process and expensive material, have higher economic nature, easily promote and use.
In order to achieve the above object, the present application provides a high performance nanofiltration membrane comprising:
first supporting layer micropore passageway, second supporting layer micropore passageway, third supporting layer micropore passageway, first supporting layer micropore passageway is close to the surface of high performance nanofiltration membrane, the third supporting layer is close to the internal surface of high performance nanofiltration membrane, just second supporting layer micropore passageway is located third supporting layer micropore passageway with between the first supporting layer micropore passageway, wherein the high performance nanofiltration membrane still has open side and holds back the side, open side with the average aperture who holds back the side is 25-250nm1-10nm respectively.
In order to realize the aim, the application provides a preparation process of a high-performance nanofiltration membrane, which comprises the following steps:
step 1: extracting spinning solution: putting 50-60 parts by mass of polyvinylidene fluoride, 3-10 parts by mass of a pore-forming agent and 50-60 parts by mass of an organic solvent into a dissolving tank, stirring for 1-2h at 80 ℃ by utilizing a forward rotation speed of a crusher for 70-80S, stirring for 60S at 80 ℃ for 60-69min at a reverse rotation speed of 55-99 r/min, mixing, crushing and stirring for 7-8h, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved to form a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 180-mesh 280-mesh filter membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.2-0.12 MPa to remove bubbles for 25-30min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially carrying out air bath curing and pre-evaporation on the primary membrane of the high-performance nanofiltration membrane obtained in the step 2 for 35-40s at the salivation temperature of 55-80 ℃ and at the salivation relative humidity of 50-55%; after primary film gas bath solidification, entering a solidification bath of 45-60% dimethyl sulfoxide DMSO aqueous solution, wherein the temperature of the solidification bath is 50-55 ℃, and the drawing ratio of a drawing godet roller is 2.5-2.9 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially subjecting the stretched and cured high-performance nanofiltration membrane primary membrane obtained in the step (3) to steam washing for 6-10min and vertical hole-preserving treatment with hole-preserving ultrasonic cleaning frequency of 70-90KHz for 12-20min, and finally air-drying at the humidity of 65-75%, the temperature of 35-45 ℃ and the time of 18-30h to prepare the high-performance nanofiltration membrane.
In one or more embodiments of the present application, the pore forming agent is formaldehyde or polyethylene glycol.
In one or more embodiments herein, the organic solvent is dimethyl sulfoxide DMSO.
In order to achieve the above object, the present application provides a direct drinking water apparatus using a high performance nanofiltration membrane, wherein the direct drinking water apparatus comprises:
a high performance nanofiltration membrane;
the shell is a cylinder penetrating through the middle of the shell, and two ends of the shell are provided with first annular bulges extending outwards;
a first rotating member including a first cylinder rotatably disposed at one end of the housing, the first cylinder having a first cavity; and
a second rotating member including a second cylinder rotatably disposed at the other end of the housing, the second cylinder having a second cavity, wherein the second cavity, the penetrating portion of the housing and the first cavity together form a receiving space, and the high-performance nanofiltration membrane is disposed in the receiving space.
In one or more embodiments of the present application, the first rotating member further includes a first limiting member and a first collar, the first cylinder is provided with a second annular protrusion on a side close to the housing, wherein one end of the first limiting member abuts against one side of the first annular protrusion deviating from the first cylinder, and the other end of the first limiting member abuts against one side of the second annular protrusion deviating from the housing, wherein the first limiting member is a ring member, and a cross-sectional shape of the first limiting member is concave, wherein the first collar is sleeved and connected to the first limiting member.
In one or more embodiments of the present application, the first rotating member further includes a first connecting plate fixedly connected to both sides of the notch of the first yoke to define the first yoke, and a first supporting member fixedly connected to the first connecting plate and configured to support an end of the housing.
In one or more embodiments of the present application, the second rotating member further includes a second limiting member and a second band, the second column is close to one side of the housing and has a third annular protrusion, wherein one end of the second limiting member abuts against another side of the first annular protrusion deviating from the second column, and the other end of the second limiting member abuts against one side of the third annular protrusion deviating from the housing, wherein the second limiting member is a ring member, and the cross-sectional shape of the second limiting member is concave, wherein the second band is sleeved and connected to the second limiting member.
In one or more embodiments of the present application, the second rotating member further includes a second connecting piece and a second supporting piece, the second connecting piece is fixedly connected to both sides of the notch of the second yoke, wherein the second supporting piece is fixedly connected to the second connecting piece, and the second supporting piece is configured to support the other end of the housing.
In one or more embodiments of this application, first cylinder deviates from one side of casing is extended there is a first arch, first arch has a first connecting hole, the second cylinder deviates from one side of casing is extended there is a second arch, the second arch has a second connecting hole, the week lateral wall of casing has a third arch, the third arch has a third connecting hole, wherein first connecting hole the third connecting hole with the third connecting hole all communicates accommodation space presses, wherein straight drinking water device still includes three sealing member, and is three the sealing member respectively rotationally connect in first arch, second arch with the third is protruding, thereby seal first connecting hole the second connecting hole with the third connecting hole.
Drawings
These and/or other aspects and advantages of the present application will become more apparent and more readily appreciated from the following detailed description of the embodiments of the present application, taken in conjunction with the accompanying drawings of which:
fig. 1 illustrates a schematic structural diagram of a direct drinking water device.
Fig. 2 and 3 are schematic structural cross-sectional views illustrating the high-performance nanofiltration membrane of the invention.
Figure 4 illustrates a high performance nanofiltration membrane structure view.
Detailed Description
The terms and words used in the following specification and claims are not limited to the literal meanings, but are used only by the inventors to enable a clear and consistent understanding of the application. Accordingly, it will be apparent to those skilled in the art that the following descriptions of the various embodiments of the present application are provided for illustration only and not for the purpose of limiting the application as defined by the appended claims and their equivalents.
It is understood that the terms "a" and "an" should be interpreted as meaning that a number of one element or element is one in one embodiment, while a number of other elements is one in another embodiment, and the terms "a" and "an" should not be interpreted as limiting the number.
While ordinal numbers such as "first," "second," etc., will be used to describe various components, those components are not limited herein. The term is used only to distinguish one element from another. For example, a first component could be termed a second component, and, similarly, a second component could be termed a first component, without departing from the teachings of the inventive concepts. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The terminology used herein is for the purpose of describing various embodiments only and is not intended to be limiting. As used herein, the singular forms are intended to include the plural forms as well, unless the context clearly indicates otherwise. It will be further understood that the terms "comprises" and/or "comprising," when used in this specification, specify the presence of stated features, numbers, steps, operations, components, elements, or combinations thereof, but do not preclude the presence or addition of one or more other features, numbers, steps, operations, components, elements, or groups thereof.
Summary of the application
There are some problems with current high performance nanofiltration membranes, such as: the high-performance nanofiltration membrane has the advantages of easy pore diameter closing, short storage time, long process flow, low porosity, short service life, low water yield and high energy consumption. In addition, the preparation process of the high-performance nanofiltration membrane has some problems, such as: the problem that the pore size of the membrane is not uniform due to nonuniform heating temperature of the materials during dissolution exists in the process of the extraction step of the spinning solution. The method comprises the following steps of post-processing and hole-keeping, wherein the problems of non-uniform film hole-keeping liquid, long film hole-keeping time and short film storage time are solved in the post-processing and hole-keeping step, the problem of serious solvent loss caused by poor defoaming time in the vacuum defoaming step is solved, and the problem of non-uniform film hole diameter forming size caused by non-uniform stress tensile strength of the inner side and the outer side of a circular winding roller and a film wire in a close contact manner is solved in the curing step. In addition, the water drinking device using the high-performance nanofiltration membrane is inconvenient to install and place due to the structural design problem, and poor in sealing performance.
Based on this, there is a need for a high-performance nanofiltration membrane, a preparation process and a direct drinking water device using the same, which can solve the above problems.
Based on the technical problem, the application provides a high performance nanofiltration membrane, preparation technology and use its straight drinking water device, wherein, high performance nanofiltration membrane, preparation technology and use its straight drinking water device simple structure do not relate to complicated manufacturing process and expensive material, have higher economic nature, simultaneously, to the producer, the high performance nanofiltration membrane that this application provided, preparation technology and use its straight drinking water device easily produces, and low cost, more be favorable to controlling manufacturing cost, further be favorable to product popularization and use.
Referring to fig. 1, the instant drinking water device using the high performance nanofiltration membrane of the present invention is described in detail below to facilitate understanding of the present invention.
Specifically, the direct drinking water apparatus includes a tank (not shown), wherein the tank includes a housing 10, a first rotating member 20 and a second rotating member 30, and the first rotating member 20 and the second rotating member 30 are rotatably connected to both ends of the housing 10.
Further, the housing 10 is shaped as a cylinder penetrating through the middle, and both ends of the housing 10 have first annular protrusions (not shown) extending outward.
Further, the first rotating member 20 includes a first retaining member 21 and a first cylinder 22, the first cylinder 22 is disposed at one end of the housing 10, and a side of the first cylinder 22 close to the housing 10 has a second annular protrusion (not shown), it is worth mentioning that, the cross-sectional diameter of the second annular projection is identical to the cross-sectional diameter of the first annular projection, wherein one end of the first retaining member 21 abuts against one side of one of the first annular protrusions facing away from the first cylinder 22, and the other end of the first limiting member 21 abuts against one side of the second annular protrusion departing from the housing 10, it should be noted that, the first limiting member 21 is an annular member, and the cross-sectional shape of the first limiting member 21 is concave, so that the first retaining member 21 defines the first cylinder 22, and the first cylinder 22 cannot move in the direction of the housing 10. It should be noted that, because the first annular protrusion and the second annular protrusion are both located between two sidewalls of the first limiting member 21, and the sum of the widths of the first annular protrusion and the second annular protrusion is smaller than the cross-sectional width of the first limiting member 21, and in addition, the heights of the first annular protrusion and the second annular protrusion are smaller than the groove depth of the first limiting member 21, the first cylinder 22 can rotate relative to the housing 10 or the housing 10 can rotate relative to the first cylinder 22.
Further, the first rotating member 20 further includes a first yoke 23, and the first yoke 23 is connected to the first limiting member 21 in a sleeved manner. The second yoke 33 is deformed by pressing, and presses the first limiting member 21, so as to limit the first limiting member 21.
Further, the first rotating member 20 further includes a first connecting tab 24, and the first connecting tab 24 is fixedly connected to both sides of the notch of the first yoke 23 to define the first yoke 23. It is worth mentioning that when the first clamp 23 is deformed by an external force, a user can manually fix the first connecting piece 24 to both sides of the notch of the first clamp 23 by an external tool to prevent the first clamp 23 from rebounding, wherein the connection manner of the first connecting piece 24 and the first clamp 23 can be implemented as a welding connection.
Further, the first rotating member 20 further includes a first supporting member 25, the first supporting member 25 is fixedly connected to the first connecting plate 24, and the first supporting member 25 is configured to support one end of the casing 10.
Further, the second rotating member 30 includes a second limiting member 31 and a second cylinder 32, the second cylinder 32 is disposed at the other end of the housing 10, and a third annular protrusion (not shown) is disposed on a side of the second cylinder 32 close to the housing 10, it is worth mentioning that, the cross-sectional diameter of the third annular projection is identical to the cross-sectional diameter of the first annular projection, wherein one end of the second limiting member 31 abuts against one side of the other first annular protrusion departing from the second cylinder 32, and the other end of the second limiting member 31 abuts against one side of the third annular protrusion departing from the housing 10, it should be noted that, the second limiting member 31 is an annular member, and the cross-sectional shape of the second limiting member 31 is concave, so that the second stopper 31 limits the second cylinder 32, and thus the second cylinder 32 cannot move in the direction of the housing 10. It should be noted that, because the first annular protrusion and the third annular protrusion are both located between two sidewalls of the second limiting member 31, and the sum of the widths of the first annular protrusion and the third annular protrusion is smaller than the cross-sectional width of the second limiting member 31, and in addition, the heights of the first annular protrusion and the third annular protrusion are smaller than the groove depth of the second limiting member 31, the second column 32 can rotate relative to the housing 10 or the housing 10 can rotate relative to the second column 32.
Further, the second rotating member 30 further includes a second yoke 33, and the second yoke 33 is connected to the second limiting member 31 in a sleeved manner. The second clip 33 is deformed by pressing, and then presses the second stopper 31, so as to limit the second stopper 31.
Further, the second rotating member 30 further includes a second connecting piece 34, and the second connecting piece 34 is fixedly connected to both sides of the notch of the second yoke 33 to define the second yoke 33. It is worth mentioning that when the second clamp 33 is deformed by an external force, a user can manually fix the second connecting piece 34 on both sides of the notch of the second clamp 33 by an external tool to prevent the second clamp 33 from rebounding, wherein the connection manner of the second connecting piece 34 and the second clamp 33 can be implemented as a welding connection.
Further, the second rotating member 30 further includes a second supporting member 35, the second supporting member 35 is fixedly connected to the second connecting piece 34, and the second supporting member 35 is configured to support the other end of the housing 10.
It should be noted that the first cylinder 22 and the second cylinder 32 respectively have a first cavity and a second cavity, wherein the first cavity, the housing 10 and the second cavity together form a containing space.
Further, a first protrusion (not shown) extends from a side of the first cylinder 22 facing away from the housing 10, and the first protrusion has a first connection hole (not shown) that communicates with the outside and the accommodating space, respectively.
Further, a second protrusion (not shown) extends from a side of the second cylinder 32 facing away from the housing 10, and the second protrusion has a second connection hole (not shown) which is respectively connected to the outside and the accommodating space.
Further, the peripheral sidewall of the housing 10 has a third protrusion 11, and the third protrusion 11 has a third connection hole (not shown) for respectively connecting the outside and the accommodation space (not shown), wherein the accommodation space is used for placing an external nanofiltration membrane. It should be noted that the axes of the first connecting hole and the second connecting hole are located on the same straight line, and the axis of the third connecting hole is perpendicular to the axes of the first connecting hole and the second connecting hole.
Specifically, the direct drinking water apparatus further includes three sealing members 40, and the three sealing members 40 are rotatably coupled to the first protrusion, the second protrusion, and the third protrusion 11, respectively, to close the first coupling hole, the second coupling hole, and the third coupling hole. It is worth mentioning that the connection of three said sealing members 40 may be implemented as a threaded connection.
It should be noted that a sealing ring (not shown) is disposed between the first cylinder 22 and the housing 10 and between the second cylinder 32 and the housing 10, so as to ensure the sealing performance of the direct drinking water device.
The preparation process of the high-performance nanofiltration membrane is explained in detail as follows:
example 1:
step 1: extracting spinning solution: putting 50 parts by mass of polyvinylidene fluoride, 3 parts by mass of a pore-forming agent and 55 parts by mass of an organic solvent into a dissolving tank, stirring for 1 hour at the forward rotation speed of 66 r/min and 80 ℃ and stopping for 70 seconds, stirring for 50 minutes at the reverse rotation speed of 66 r/min and 80 ℃ and stopping for 60 seconds, mixing, crushing and stirring for 7 hours, and fully dissolving and swelling until the materials are completely dissolved into a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 180-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.2 MPa for pretreatment of removing bubbles for 25min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the high-performance nanofiltration membrane primary membrane obtained in the step (2) through air bath curing and pre-evaporation for 35s at the salivation temperature of 55 ℃ and at the salivation relative humidity of 50%; after primary film gas bath solidification, entering a solidification bath 45% dimethyl sulfoxide DMSO aqueous solution, at the solidification bath temperature of 50 ℃, and drawing by 2.5 times of draw ratio of a draw godet roller for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) with steam for 6min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol at a pore-preserving ultrasonic frequency of 70KHz, vertically preserving pores for 12min, and finally air-drying at a humidity of 65%, a temperature of 35 ℃ and a temperature of 18h to prepare the high-performance nanofiltration membrane.
Example 2:
step 1: extracting spinning solution: putting 55 parts by mass of polyvinylidene fluoride, 12 parts by mass of a pore-forming agent and 60 parts by mass of an organic solvent into a dissolving tank, stirring for 2 hours at a forward rotation speed of 99 revolutions/min and 80 ℃ and stopping for 80 seconds at a reverse rotation speed of 99 revolutions/min and 80 ℃ for 50 minutes and stopping for 60 seconds, mixing, crushing and stirring for 8 hours, and fully dissolving and swelling until the materials are completely dissolved into a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 280-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.12 MPa to remove bubbles for 30min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the high-performance nanofiltration membrane primary membrane obtained in the step (2) through air bath curing and pre-evaporation for 40s at the salivation temperature of 80 ℃ and at the salivation relative humidity of 55%; after primary film gas bath solidification, the film enters a coagulation bath 60% dimethyl sulfoxide DMSO aqueous solution, the temperature of the coagulation bath is 55 ℃, and the drawing ratio of a drawing godet roller is 2.9 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) with steam for 10min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol pore-preserving ultrasonic frequency of 90KHz, vertically preserving pores for 20min, and finally air-drying at the humidity of 75%, the temperature of 45 ℃ and 30h to prepare the high-performance nanofiltration membrane.
Example 3:
step 1: extracting spinning solution: putting 58 parts by mass of polyvinylidene fluoride, 10 parts by mass of a pore-forming agent and 58 parts by mass of an organic solvent into a dissolving tank, stirring for 2 hours and 60 seconds at a forward rotation speed of 99 revolutions/min and 80 ℃ and stopping stirring for 60 seconds at a reverse rotation speed of 99 revolutions/min and 80 ℃, and stirring for 60 minutes and 60 seconds at a reverse rotation speed of 99 revolutions/min and 80 ℃, mixing, crushing and stirring for 8 hours, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved to form a;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 280-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.15 MPa to remove bubbles for 28min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the high-performance nanofiltration membrane primary membrane obtained in the step (2) through air bath curing and pre-evaporation for 40s at the salivation temperature of 60 ℃ and at the salivation relative humidity of 55%; after primary film gas bath solidification, entering a solidification bath 45% dimethyl sulfoxide DMSO aqueous solution, at the solidification bath temperature of 50 ℃, and drawing by 2.7 times of drawing ratio of a draw godet roller for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the high-performance nanofiltration membrane primary membrane stretched and cured in the step (3) with steam for 10min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol pore-preserving ultrasonic frequency of 70KHz, vertically preserving pores for 15min, and finally air-drying at the humidity of 65%, the temperature of 45 ℃ and the temperature of 30h to prepare the high-performance nanofiltration membrane.
Example 4:
step 1: extracting spinning solution: putting 50 parts by mass of polyvinylidene fluoride, 4 parts by mass of a pore-forming agent and 60 parts by mass of an organic solvent into a dissolving tank, stirring for 2 hours at a forward rotation speed of 55 r/min and 80 ℃ and stopping for 80 seconds at a reverse rotation speed of 55 r/min and 80 ℃ and stopping for 60 seconds at a reverse rotation speed of 69 minutes, mixing, crushing and stirring for 7 hours, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved to form a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 280-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.13 MPa for pretreatment of removing bubbles for 25min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the high-performance nanofiltration membrane primary membrane obtained in the step (2) through air bath curing and pre-evaporation for 35s at the salivation temperature of 55 ℃ and at the salivation relative humidity of 55%; after primary film gas bath solidification, entering a solidification bath 45% dimethyl sulfoxide DMSO aqueous solution, at the solidification bath temperature of 50 ℃, and drawing by 2.5 times of draw ratio of a draw godet roller for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) with steam for 6min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol at a pore-preserving ultrasonic frequency of 70KHz, vertically preserving pores for 12min, and finally air-drying at a humidity of 65%, a temperature of 35 ℃ and a temperature of 18h to prepare the high-performance nanofiltration membrane.
Example 5:
step 1: extracting spinning solution: putting 35 parts by mass of polyvinylidene fluoride, 6 parts by mass of a pore-forming agent and 55 parts by mass of an organic solvent into a dissolving tank, stirring for 1.5 hours at 80 ℃ by using a crusher at a forward rotation speed of 80 r/min for stopping for 75S, stirring for 69 minutes at 80 ℃ at a reverse rotation speed of 80 r/min for stopping for 60S, mixing, crushing and stirring for 7.5 hours, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved to form a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 250-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.14 MPa to remove bubbles for 30min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the primary membrane of the high-performance nanofiltration membrane obtained in the step 2 through air bath curing and pre-evaporation for 40s at the salivation temperature of 70 ℃ and at the salivation relative humidity of 55%; after primary film gas bath solidification, the primary film enters a 58% dimethyl sulfoxide DMSO aqueous solution in a coagulation bath, the temperature of the coagulation bath is 53 ℃, and the drawing ratio of a drawing godet roller is 2.6 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the high-performance nanofiltration membrane primary membrane stretched and cured in the step (3) with steam for 8min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol pore-preserving ultrasonic frequency of 88KHz, vertically preserving pores for 15min, and finally air-drying at the humidity of 70%, the temperature of 44 ℃ and 24h to prepare the high-performance nanofiltration membrane.
Example 6:
step 1: extracting spinning solution: putting 50 parts by mass of polyvinylidene fluoride, 4 parts by mass of a pore-forming agent and 60 parts by mass of an organic solvent into a dissolving tank, stirring for 1.5 hours at a forward rotation speed of 60 r/min and 80 ℃ by using a crusher, stopping stirring for 75 seconds, stirring for 60 minutes at a reverse rotation speed of 60 r/min and 80 ℃ for 60 seconds, mixing, crushing and stirring for 7 hours, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved into a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 260-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.16 MPa for pretreatment of removing bubbles for 25min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the high-performance nanofiltration membrane primary membrane obtained in the step (2) through air bath curing and pre-evaporation for 35s at the salivation temperature of 60 ℃ and at the salivation relative humidity of 55%; after primary film gas bath solidification, entering a solidification bath 45% dimethyl sulfoxide DMSO aqueous solution, wherein the temperature of the solidification bath is 55 ℃, and the drawing ratio of a drawing godet roller is 2.8 times of that of the solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the high-performance nanofiltration membrane primary membrane stretched and cured in the step (3) with steam for 6min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol pore-preserving ultrasonic frequency of 75KHz, vertically preserving pores for 13min, and finally air-drying at the humidity of 66%, the temperature of 36 ℃ and the time of 16h to prepare the high-performance nanofiltration membrane.
Example 7:
step 1: extracting spinning solution: putting 55 parts by mass of polyvinylidene fluoride, 2 parts by mass of a pore-forming agent and 50 parts by mass of an organic solvent into a dissolving tank, stirring for 1 hour at the forward rotation speed of 58 r/min and the temperature of 80 ℃ and stopping for 60 seconds, stirring for 60 minutes at the reverse rotation speed of 58 r/min and the temperature of 80 ℃ and stopping for 60 seconds, mixing, crushing and stirring for 8 hours, and fully dissolving and swelling until the materials are completely dissolved into a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 200-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.13 MPa to remove bubbles for 28min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially passing the primary membrane of the high-performance nanofiltration membrane obtained in the step 2 through air bath curing and pre-evaporation for 40s, wherein the salivation temperature is 75 ℃ and the salivation relative humidity is 55%; after primary film gas bath solidification, the primary film enters a coagulating bath 53% dimethyl sulfoxide DMSO aqueous solution, the temperature of the coagulating bath is 50 ℃, and the drawing ratio of a drawing godet roller is 2.9 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) with steam for 6min, cleaning with a pore-preserving agent Mg (ClO4)2 or polyethylene glycol at a pore-preserving ultrasonic frequency of 70KHz, vertically preserving pores for 12min, and finally air-drying at a humidity of 65%, a temperature of 35 ℃ and a temperature of 18h to prepare the high-performance nanofiltration membrane.
Example 8:
step 1: extracting spinning solution: putting 50 parts by mass of polyvinylidene fluoride, 6 parts by mass of a pore-forming agent and 50 parts by mass of an organic solvent into a dissolving tank, stirring for 2 hours at the forward rotation speed of 77 r/min and 80 ℃ and stopping for 60 seconds, stirring for 69 minutes at the reverse rotation speed of 77 r/min and 80 ℃ and stopping for 60 seconds by utilizing a crusher, mixing, crushing and stirring for 7.5 hours, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved into a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 280-mesh filtering membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.18 MPa to remove bubbles for 30min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially carrying out air bath curing and pre-evaporation on the primary membrane of the high-performance nanofiltration membrane obtained in the step 2 for 10s at the salivation temperature of 80 ℃ and at the salivation relative humidity of 22%; after primary film gas bath solidification, the film enters a coagulation bath 60% dimethyl sulfoxide DMSO aqueous solution, the temperature of the coagulation bath is 55 ℃, and the drawing ratio of a drawing godet roller is 2.9 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially washing the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) with steam for 10min, cleaning with a pore-preserving agent formaldehyde or polyethylene glycol at a pore-preserving ultrasonic frequency of 90KHz, vertically preserving pores for 20min, and finally air-drying at a humidity of 75%, a temperature of 45 ℃ and a temperature of 30h to prepare the high-performance nanofiltration membrane.
Referring to fig. 2 to 4, the high-performance nanofiltration membrane a has a first nanoscale pore surface; b, a first support layer micropore channel; c, a second support layer micropore channel; d a body interposed between the surfaces of the first and second support layers; e a second nanoscale pore surface; f, a third support layer micropore channel; the high-performance nanofiltration membrane has an open side and a cut-off side, and the average pore diameters are respectively 25-250nm and 1-10 nm; when the filter works, the filter operates under the internal pressure of 0.2MPa at the ultralow pressure, low-molecular organic matters and bacterial viruses are removed through the surface of a first nano-scale pore diameter of 25-250nm, the filter enters a first support layer finger-shaped micropore channel B, 5nm substances are removed through a nano-scale pore diameter of 1-10nm between a first support body and a second support body of a filtrate D, and the filtrate sequentially passes through a second support layer micropore channel C, a third support layer micropore channel F and a second nano-scale pore diameter E to finish the internal pressure type filtration. During backwashing, external pressure type operation is performed under the ultralow pressure of 0.2MPa, and impurities are washed away from the inner wall sequentially through the E second nano-scale aperture, the F third supporting layer microporous channel, the C second supporting layer microporous channel, the D nano-scale aperture between the first supporting body and the second supporting body, the B first supporting microporous channel and the A first nano-scale aperture. The service life of the high-performance nanofiltration membrane is prolonged by 5-10 years. The special structure improves the pollution resistance. F, nano-scale holes between the first support and the second support are 1-10 nm. And the microporous channels of the three support layers enhance the compression resistance of the membrane.
The high-performance nanofiltration membrane prepared by the method scans the distribution and size of the pore diameters of each compact layer and the supporting layer of the high-performance nanofiltration membrane through an electron microscope. The high-performance nanofiltration membrane has the advantages that the storage time of the high-performance nanofiltration membrane is more than 15 years, the pore size, the porosity and the water flux are not changed, and the improved pore-preserving process is used for uniformly entering the pore size to avoid pore closing. The high-performance nanofiltration membrane and the composite nanofiltration membrane are simultaneously applied to tap water and sewage for 5 to 10 years, and the flux of the composite nanofiltration membrane is reduced by 40 to 70 percent after the composite nanofiltration membrane is operated for 1 to 2 years. The flux of the high-performance nanofiltration membrane is reduced by 10-20% and then is recovered to 90% through back pressure washing. The industrial production does not need to be compounded by polyhydric alcohol and acyl chloride, and the process innovation combines positive rotation and reverse rotation by a crushing motor, so that the material is heated uniformly, and the material dissolving time is shortened; the unit problems of different membrane aperture sizes and shapes caused by uneven stress on two sides of the same membrane yarn are solved by adopting a positive-negative guide wire, a positive-negative stretching and polygonal swinging needle type flat plate winding; a deaeration tank drainage rod is adopted to enter the inner wall of the device, so that the bubbles of the spinning solution are reduced, the deaeration time is shortened, and the loss of the solvent is reduced; the ultrasonic wave principle is used for converting sound energy of a power ultrasonic frequency source into mechanical vibration, so that micro bubbles in liquid in a tank can keep vibrating under the action of the sound wave, the membrane pore-protecting liquid is uniform, the membrane pore-protecting time is shortened, the storage time of the membrane is prolonged, the working efficiency is improved, the production cost is reduced, and the energy conservation and emission reduction are realized.
It will be appreciated by persons skilled in the art that the embodiments of the invention described above and shown in the drawings are given by way of example only and are not limiting of the invention. The objects of the invention have been fully and effectively accomplished. The functional and structural principles of the present invention have been shown and described in the examples, and any variations or modifications of the embodiments of the present invention may be made without departing from the principles.
Claims (10)
1. A high performance nanofiltration membrane, comprising: first supporting layer micropore passageway, second supporting layer micropore passageway, third supporting layer micropore passageway, first supporting layer micropore passageway is close to the surface of high performance nanofiltration membrane, the third supporting layer is close to the internal surface of high performance nanofiltration membrane, just second supporting layer micropore passageway is located third supporting layer micropore passageway with between the first supporting layer micropore passageway, wherein the high performance nanofiltration membrane still has open side and holds back the side, open side with the average aperture who holds back the side is 25-250nm1-10nm respectively.
2. A process for preparing a high-performance nanofiltration membrane, which is used for the high-performance nanofiltration membrane of claim 1, and comprises the following steps:
step 1: extracting spinning solution: putting 50-60 parts by mass of polyvinylidene fluoride, 3-10 parts by mass of a pore-forming agent and 50-60 parts by mass of an organic solvent into a dissolving tank, stirring for 1-2h at 80 ℃ by utilizing a forward rotation speed of a crusher for 70-80S, stirring for 60S at 80 ℃ for 60-69min at a reverse rotation speed of 55-99 r/min, mixing, crushing and stirring for 7-8h, and fully dissolving and swelling until the polyvinylidene fluoride, the pore-forming agent and the organic solvent are completely dissolved to form a spinning solution;
step 2: spinning: removing impurities from the spinning solution obtained in the step 1 through a 180-mesh 280-mesh filter membrane, and then introducing the spinning solution into a vacuum defoaming device with the vacuum degree of-0.2-0.12 MPa to remove bubbles for 25-30min at the temperature of 80 ℃; preparing the pretreated impurity-free and bubble-free spinning solution into a high-performance nanofiltration membrane primary membrane by a dry-jet wet spinning method;
and step 3: and (3) curing: sequentially carrying out air bath curing and pre-evaporation on the primary membrane of the high-performance nanofiltration membrane obtained in the step 2 for 35-40s at the salivation temperature of 55-80 ℃ and at the salivation relative humidity of 50-55%; after primary film gas bath solidification, entering a solidification bath of 45-60% dimethyl sulfoxide DMSO aqueous solution, wherein the temperature of the solidification bath is 50-55 ℃, and the drawing ratio of a drawing godet roller is 2.5-2.9 times for drawing solidification;
and 4, step 4: post-treatment and hole protection: and (3) sequentially subjecting the primary membrane of the high-performance nanofiltration membrane stretched and cured in the step (3) to steam washing for 6-10min and vertical hole-preserving treatment with hole-preserving ultrasonic cleaning frequency of 70-90KHz for 12-20min, and finally air-drying at the humidity of 65-75%, the temperature of 35-45 ℃ and the time of 18-30h to prepare the high-performance nanofiltration membrane.
3. The preparation process of the high-performance nanofiltration membrane according to claim 2, wherein the pore-forming agent is formaldehyde or polyethylene glycol.
4. The preparation process of the high-performance nanofiltration membrane according to claim 2, wherein the organic solvent is dimethyl sulfoxide (DMSO).
5. The utility model provides an use straight drinking water device of high performance nanofiltration membrane, includes a jar body, its characterized in that jar body includes:
a high performance nanofiltration membrane of claims 1 to 2;
the shell is a cylinder penetrating through the middle of the shell, and two ends of the shell are provided with first annular bulges extending outwards;
a first rotating member including a first cylinder rotatably disposed at one end of the housing, the first cylinder having a first cavity; and
a second rotating member including a second cylinder rotatably disposed at the other end of the housing, the second cylinder having a second cavity, wherein the second cavity, the penetrating portion of the housing and the first cavity together form a receiving space, and the high-performance nanofiltration membrane is disposed in the receiving space.
6. A drinking water device according to claim 5, wherein the first rotation member further includes a first stopper and a first collar, one side of the first cylinder near the housing has a second annular protrusion, wherein one end of the first stopper abuts against one side of one of the first annular protrusions facing away from the first cylinder, and the other end of the first stopper abuts against one side of the second annular protrusion facing away from the housing, wherein the first stopper is a ring-shaped member, and the first stopper has a concave cross-sectional shape, wherein the first collar is sleeved and connected to the first stopper.
7. A drinking water device according to claim 6, wherein the first rotation member further includes a first connecting piece and a first support piece, the first connecting piece is fixedly connected to both sides of the notch of the first yoke to define the first yoke, wherein the first support piece is fixedly connected with the first connecting piece, and the first support piece is configured to support one end of the housing.
8. A drinking water device according to claim 7, wherein the second rotation member further includes a second stopper and a second collar, a third annular protrusion is provided on a side of the second column near the housing, wherein one end of the second stopper abuts against another side of the first annular protrusion facing away from the second column, and the other end of the second stopper abuts against a side of the third annular protrusion facing away from the housing, wherein the second stopper is an annular member, and the cross-sectional shape of the second stopper is concave, wherein the second collar is coupled to the second stopper.
9. A drinking water device according to claim 8, wherein the second rotation member further includes a second connecting piece and a second support piece, the second connecting piece is fixedly connected to both sides of the notch of the second yoke, wherein the second support piece is fixedly connected to the second connecting piece, and the second support piece is configured to support the other end of the housing.
10. A direct drinking water device according to claim 9, wherein a first protrusion extends from a side of said first column body facing away from said housing, said first protrusion has a first connection hole, a second protrusion extends from a side of said second column body facing away from said housing, said second protrusion has a second connection hole, a peripheral sidewall of said housing has a third protrusion, said third protrusion has a third connection hole, wherein said first connection hole, said third connection hole and said third connection hole all communicate with said receiving space, wherein said direct drinking water device further comprises three sealing members, three of said sealing members are rotatably connected to said first protrusion, said second protrusion and said third protrusion, respectively, thereby closing said first connection hole, said second connection hole and said third connection hole.
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| CN205850611U (en) * | 2016-06-27 | 2017-01-04 | 南京九思高科技有限公司 | A kind of clamping hoop type inorganic antibacterial film water purifier |
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