CN111054220B - Drying method of organic tubular membrane - Google Patents
Drying method of organic tubular membrane Download PDFInfo
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- CN111054220B CN111054220B CN201911392560.5A CN201911392560A CN111054220B CN 111054220 B CN111054220 B CN 111054220B CN 201911392560 A CN201911392560 A CN 201911392560A CN 111054220 B CN111054220 B CN 111054220B
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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
- B01D69/04—Tubular membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0081—After-treatment of organic or inorganic membranes
- B01D67/0095—Drying
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/08—Humidity
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
- F26B21/06—Controlling, e.g. regulating, parameters of gas supply
- F26B21/10—Temperature; Pressure
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B9/00—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards
- F26B9/06—Machines or apparatus for drying solid materials or objects at rest or with only local agitation; Domestic airing cupboards in stationary drums or chambers
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
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Abstract
The invention discloses a drying method of an organic tubular membrane, which comprises the following steps: s1, draining: transferring the organic tubular membrane solidified and formed in the coagulating bath into pure water for soaking, and then taking out and draining the water on the surface of the organic tubular membrane; s2, drying: placing the drained organic tubular membrane in a constant-temperature constant-humidity box, and drying in a high-temperature high-humidity environment; s3, primary dehumidification: keeping the temperature unchanged, reducing the humidity by 5-10% and drying; s4, primary cooling: keeping the humidity unchanged, and reducing the drying temperature of the organic tubular membrane in primary dehumidification by 5-20 ℃; s5, circulating S3 and S4 at least twice; s6, drying: the organic tubular membrane obtained in S5 was subjected to a dehumidifying operation until a humidity of less than 40% was reached. Through using the constant temperature and humidity box to dry the organic tubular membrane in sections, the process is simplified, the membrane is not required to be pretreated by post-treatment liquid and then dried, the residue of components in the treatment liquid in the membrane is avoided, the production cost is reduced, and the production efficiency is improved.
Description
Technical Field
The invention belongs to the technical field of organic separation membranes, and particularly relates to a drying method of an organic tubular membrane.
Background
The membrane technology is a separation technology with low energy consumption and low cost because of low energy consumption, and the membrane separation device is simple, easy to operate, convenient to manufacture and easy to combine with other separation technologies, so that the membrane technology has wide application in many fields.
The membrane device is composed of a plurality of different membrane components, the membrane components are the core of the membrane device, and the membrane components are in the forms of spiral-wound membrane components, flat-plate membrane components, hollow fiber membrane components, tubular membrane components and the like. The tubular membrane component has simple structure, is not easy to block and clean, and can treat high-viscosity and high-solid feed liquid. The organic tubular membrane wet membrane is difficult to store and transport, and is difficult to be made into a membrane component, and generally made into a dry membrane. At present, organic tubular membranes are mostly prepared by a non-solvent induced phase separation method, and are solidified and formed in water or a coagulating bath consisting of water and other solvents or non-solvents, and the formed organic tubular membranes are further treated by various post-treatment liquids and then are correspondingly dried, so that membrane pores are ensured not to collapse, and the reduction of permeability is reduced.
In U.S. Pat. No. US5385670A, a drying method for porous ultrafiltration membranes is disclosed, in which a water-soluble organic solid is dissolved in an organic solvent to treat the membrane, and then the membrane is dried, the organic solvent is volatilized, and the organic solid remains in the membrane pores to ensure that the membrane pores are not collapsed. In european patent publication No. EP1466659a1, a method of drying a wet porous membrane and a porous membrane structure obtained by the method are disclosed, an organic tubular membrane is immersed in an aqueous solution of calcium chloride and then dried. A preparation method of a strong acid and strong base resistant polyether sulfone tubular ultrafiltration dry film is disclosed in Chinese patent publication No. CN201210474461, and comprises the steps of soaking a tubular ultrafiltration membrane wet film in a membrane dry-state treatment liquid, and naturally airing or drying to obtain the tubular dry film.
The process has the defects of complex process, long production period, organic or inorganic substance residue in the film, and the need of adding an additional treatment process for removal before use, can not be directly applied, and also additionally increases the production cost of enterprises.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide a drying method of an organic tubular membrane, which solves the technical problems in the prior art.
The purpose of the invention can be realized by the following technical scheme:
a method of drying an organic tubular membrane comprising the steps of:
s1, draining: transferring the organic tubular membrane solidified and formed in the coagulating bath into pure water to be soaked for 1-3 days, and then taking out the membrane to drain the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
s2, drying: placing the drained organic tubular membrane in a constant temperature and humidity box, and drying for 10-60min under the environment that the temperature is more than or equal to 60 ℃ and the humidity is more than 60%; (ii) a
S3, primary dehumidification: keeping the temperature unchanged, reducing the humidity by 5-10%, and drying for 10-60 min;
s4, primary cooling: keeping the humidity unchanged, reducing the drying temperature of the organic tubular membrane in the primary dehumidification by 5-20 ℃, and staying for 10-60 min;
s5, circulating S3 and S4 for at least two times until the environmental temperature of the organic tubular membrane is less than or equal to 30 ℃ and the humidity is 40-60%;
s6, drying: carrying out dehumidification operation on the organic tubular membrane obtained in the step S5 until the humidity is less than 40%, and obtaining a dry organic tubular membrane;
wherein: the membrane flux change rate of the organic tubular membrane is less than 5%.
Further, the temperature of the pure water in S1 was 35 ℃.
Further, the organic tubular membrane in S1 is made of: one of polyaryletherketone, polyvinylidene fluoride, polyethersulfone, polysulfone and polyvinyl chloride.
Further, the diameter of the cured and formed organic tubular membrane in the S1 is 5-25 mm.
Further, when the S2 organic tubular membranes are placed, each group of organic tubular membranes are placed in a single layer mode, so that each membrane tube is fully dried and dried uniformly.
Furthermore, when the organic tubular membrane in the S6 is subjected to dehumidification, the ambient temperature is kept to be less than or equal to 30 ℃.
Further, when the humidity in the S6 is reduced, the humidity of the organic tubular membrane is reduced by 1-5% every 5-20 min.
Further, the membrane flux change rate of the dried organic tubular membrane after the S6 treatment is controlled within 5%.
The invention has the beneficial effects that:
1. the organic tubular membrane is dried by the constant temperature and humidity box in sections, so that the process is simplified, the membrane is not required to be pretreated by post-treatment liquid and then dried, the components of the treatment liquid are prevented from remaining in the organic tubular membrane during treatment, the production cost is reduced, and the production efficiency is improved.
2. Through the sectional temperature and humidity control drying, the change of the membrane flux after drying is very small, compared with the natural drying process, the invention has the advantages of simple process and controllable conditions, and the membrane pores of the tubular membrane which is not subjected to humidity control drying are seriously collapsed and the flux attenuation is large.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to 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.
Example 1:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PEK (polyaryletherketone) organic tubular membrane solidified and formed in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 3 days, and taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
wherein can also adopt the material selection with organic tubular membrane as required to be: polyvinylidene fluoride (PVDF), Polyethersulfone (PES), Polysulfone (PSF), polyvinyl chloride (PVC). The diameter of the film tube formed by curing the organic tubular film is 6 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 1.
S3, drying: and (3) when the ambient temperature is equal to 30 ℃, carrying out dehumidification operation until the humidity is less than 40%, thus obtaining the dry organic tubular membrane.
TABLE 1
Example 2:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PVDF (polyvinylidene fluoride) organic tubular membrane solidified and molded in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 1 day, and then taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 8 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 2.
S3, drying: and (3) when the ambient temperature is 10 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 2
Example 3:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PES (polyether sulfone) organic tubular membrane solidified and formed in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ to be soaked for 2 days, and then taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 10 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 3.
S3, drying: and (3) when the ambient temperature is 10 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 3
Example 4:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PVC (polyvinyl chloride) organic tubular membrane cured and formed in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 2 days, and then taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 25 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 4.
S3, drying: and (3) when the ambient temperature is 10 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 4
Example 5:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PEK (polyaryletherketone) organic tubular membrane solidified and formed in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 2 days, and taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 8 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 5.
S3, drying: and (3) when the ambient temperature is 20 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 5
Example 6:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PVDF (polyvinylidene fluoride) organic tubular membrane solidified and molded in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 3 days, and then taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 12 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 6.
S3, drying: and (3) when the ambient temperature is 20 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 6
Example 7:
the embodiment provides a drying method of an organic tubular membrane, which comprises the following steps:
s1, draining: transferring the PVDF (polyvinylidene fluoride) organic tubular membrane solidified and molded in the coagulating bath into pure water (with residual solvent removed) at the temperature of 35 ℃ for soaking for 3 days, and then taking out and draining the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
the diameter of the film tube formed by curing the organic tubular film is 8 mm.
S2, segmented drying: and (3) placing the drained organic tubular membranes in a constant temperature and humidity box, wherein each group of organic tubular membranes are placed in a single layer mode during placement, and performing segmented drying, wherein the specific drying state is shown in table 7.
S3, drying: and (3) when the ambient temperature is 30 ℃, carrying out dehumidification operation until the humidity is less than 40%, and obtaining the dried organic tubular membrane.
TABLE 7
Comparative example 1: the PEK (polyaryletherketone) organic tubular membrane with the diameter of 6mm cured and formed in the coagulating bath is transferred to pure water with the temperature of 35 ℃ for soaking for 3 days, then is placed into 40 wt% glycerol aqueous solution for soaking for 2 days, and then is taken out and placed on a membrane tube storage rack to be naturally dried for 3 days. The film tube storage rack is placed indoors at the room temperature of 25 +/-5 ℃ and the humidity of 40-60%.
Comparative example 2: the PEK (polyaryletherketone) organic tubular membrane with the diameter of a membrane tube being 6mm and solidified and formed in a coagulating bath is transferred into pure water with the temperature of 35 ℃ for soaking for 3 days, and then the membrane is taken out to drain the water on the surface. The membrane tube drained of moisture was placed in a drying oven. The membrane tube used the staged drying process as shown in table 8 below, with each stage being run at a different temperature.
TABLE 8
The membrane pores may be shrunk according to the drying process of the membrane, resulting in a decrease in pure water flux.
The pure water flux of the tubular membranes of the examples and comparative examples was tested at a temperature of 25 c and a pressure of 0.1MPa, while the flux of the wet membranes before drying of the examples and comparative examples was tested for comparison. The test results are given in table 9 below:
TABLE 9
| Wet membrane flux (L/m)2·h) | Dry film flux (L/m)2·h) | Rate of change of flux | |
| Example 1 | 1200 | 1150 | -4.2％ |
| Example 2 | 1500 | 1460 | -2.7％ |
| Example 3 | 400 | 380 | -5.0％ |
| Example 4 | 800 | 760 | -5.0％ |
| Example 5 | 1200 | 1220 | 1.7％ |
| Example 6 | 1500 | 1490 | -0.7％ |
| Example 7 | 1500 | 1550 | 3.3％ |
| Comparative example 1 | 1200 | 1210 | 0.8％ |
| Comparative example 2 | 1200 | 100 | -91.7％ |
It can be seen from table 9 that by means of the stepwise temperature and humidity controlled drying, the flux change of the dried membrane is controlled within 5% very little, and compared with the natural drying process, the drying process has the advantages of simple process and controllable conditions, and the membrane pores of the tubular membrane which is not subjected to humidity controlled drying are seriously collapsed and the flux attenuation is large.
In conclusion, the organic tubular membrane is dried by the constant temperature and humidity box in sections, so that the process is simplified, the membrane is not required to be dried after being pretreated by the post-treatment liquid, the components of the post-treatment liquid are prevented from remaining in the organic tubular membrane during treatment, the production cost is reduced, and the production efficiency is improved.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed.
Claims (5)
1. A drying method of an organic tubular membrane is characterized by comprising the following steps:
s1, draining: transferring the organic tubular membrane solidified and formed in the coagulating bath into pure water to be soaked for 1-3 days, and then taking out the membrane to drain the water on the surface of the organic tubular membrane to obtain a drained organic tubular membrane;
s2, drying: placing the drained organic tubular membrane in a constant temperature and humidity box, and drying for 10-60min under the environment that the temperature is more than or equal to 60 ℃ and the humidity is more than 60%;
s3, primary dehumidification: keeping the temperature unchanged, reducing the humidity by 5-10%, and drying for 10-60 min;
s4, primary cooling: keeping the humidity unchanged, reducing the drying temperature of the organic tubular membrane in the primary dehumidification by 5-20 ℃, and staying for 10-60 min;
s5, circulating S3 and S4 for at least two times until the temperature of the organic tubular membrane is less than 30 ℃ and the humidity is 40-60%;
s6, drying: carrying out dehumidification operation on the organic tubular membrane obtained in the step S5 until the humidity is less than 40%, and obtaining a dry organic tubular membrane;
wherein: the membrane flux change rate of the organic tubular membrane is less than 5 percent;
when the organic tubular membrane in the S6 is subjected to dehumidification, the environmental temperature is kept to be less than or equal to 30 ℃; and when the S6 is subjected to dehumidification, reducing the humidity of the organic tubular membrane by 1-5% every 5-20 min.
2. The method for drying an organic tubular membrane according to claim 1, wherein the temperature of the pure water in S1 is 35 ℃.
3. The method for drying an organic tubular membrane according to claim 1, wherein the organic tubular membrane in S1 is made of: one of polyaryletherketone, polyvinylidene fluoride, polyethersulfone, polysulfone and polyvinyl chloride.
4. The method for drying an organic tubular film according to claim 3, wherein the cured organic tubular film in S1 has a diameter of 5-25 mm.
5. The method for drying an organic tubular film according to claim 1, wherein each group of the S2 organic tubular films is arranged in a single layer.
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