CN107824056A - A kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane - Google Patents
A kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane Download PDFInfo
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- CN107824056A CN107824056A CN201711164128.1A CN201711164128A CN107824056A CN 107824056 A CN107824056 A CN 107824056A CN 201711164128 A CN201711164128 A CN 201711164128A CN 107824056 A CN107824056 A CN 107824056A
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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
- B01D71/02—Inorganic material
- B01D71/021—Carbon
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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
- B01D67/0039—Inorganic membrane manufacture
- B01D67/0067—Inorganic membrane manufacture by carbonisation or pyrolysis
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/24—Mechanical properties, e.g. strength
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Abstract
The invention discloses a kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane, it is characterized in that using cheap waste and old aromatic polyamide reverse osmosis membrane as raw material, it is cleaned by ultrasonic, dry in the shade, preservation flattens between being placed in graphite cake, the waste and old aromatic polyamide reverse osmosis membrane close adhesion of two panels is made using adhesive and pore size control agent composition, carbonized, by the addition and carbonization condition that control adhesive and pore size control agent, preparation has different average pore diameters and pore-size distribution, pore structure is flourishing, the good carbon molecular sieve membrance of separating property.The present invention solves the problems such as carbon molecular sieve membrance prepares higher cost, complex process, organic solvent pollution, provide a kind of low cost, simple production process, be easy to industrialization, the preparation method of free of contamination carbon molecular sieve membrance, available for the carbon molecular sieve membrance for preparing different separation requirements, while also solves the solid waste pollution problem of waste and old aromatic polyamide reverse osmosis membrane.
Description
Technical field:
The present invention relates to a kind of preparation method of carbon molecular sieve membrance, more particularly to a kind of waste and old aromatic polyamide reverse osmosis membrane
The method for preparing carbon molecular sieve membrance, belongs to new material technology field.
Background technology:
In recent years, osmosis filtration technology because its have normal temperature, without phase transformation, energy consumption is low, floor space is small, non-environmental-pollution, suitable
With water quality it is wide the advantages that, since the advent of the world just enjoys industry to favor, and quick development has been obtained, particularly in recent years in water resource
Famine, water pollution, environmental pollution are serious, sewage disposal, purification of water quality etc. there is an urgent need to and government policy support situation
Under, reverse osmosis technology has obtained high speed development, is widely used in boiler feedwater, industrial pure water, desalinization, municipal water supply
With sewage treatment area, also obtained in multiple industrial trades such as oil, electric power, metallurgy, chemical industry, electronics, pharmacy, food fully
Development, turns into important energy-efficient Engineering operation unit, realizes the important component of the strategy of sustainable development.
The reverse-osmosis membrane element that the whole world produces every year has several hundred million, and the Chinese reverse osmosis membrane market demand is wide, rough estimates, disappears
The amount of receiving accounts for the whole world 10%, and is rising year by year, according to the insiders analysis prediction, and China's film market demand will be with annual 20% or so
Speed increase.But reverse osmosis membrane, in separation process, easily contaminated or mechanical damage, causes its clearance and aquifer yield
Significantly decline, lead to not efficiency of bringing into normal play, its service life is usually 2-3 or so, belongs to easily-consumed products.Therefore,
The country there are about millions of membrane components and gone out of use because of hydraulic performance decline every year, and going from strength to strength with counter-infiltration market, this
Data are constantly being refreshed.These discarded reverse osmosis membranes are because its material can hardly be degraded under field conditions (factors), if place
It is improper to put, and not only pollutes environment and wastes resource.How to dispose the waste and old reverse osmosis membrane of this substantial amounts turns into industry
A great problem.
At present, there are two kinds for discarding the common processing mode of reverse osmosis membrane, first, as solid waste refuse disposal, this side
Method not only increases environmental pressure, adds offal treatment cost, while waste resource;Second, fraction is made profits again
With also having many unit or individuals for receiving and selling second-hand film on the market at present, it is notable that regeneration membrane industry often goes out
New, shoddy dirty pool now is rushed with old, and the reverse osmosis membrane service life after regeneration is short, must finally be used as solid
Useless refuse disposal, the shortcomings that both processing methods are all present clearly.Waste and old aromatic polyamide reverse osmosis membrane, due to residual
Charcoal amount is high, is the excellent presoma for preparing carbon molecular sieve, realizes the resource reutilization system of waste and old aromatic polyamide reverse osmosis membrane
Standby carbon molecular sieve, not only reduces the quantity of waste and old reverse osmosis membrane, reduces the processing cost of waste and old reverse osmosis membrane, be that one kind has
The processing mode of effect, while policy requirements of the country on changing rejected material to useful resource are also complied with, therefore, discard the outlet of reverse osmosis membrane
Key is in resource reutilization.
At present, the production of carbon molecular sieve membrance mostly prepares precursor film using solvent method, and this method is required for the solvent of costliness
Raw material is done, polymeric membrane is prepared come evaporation solvent by pyroprocess, this method all right and wrong in terms of resource or the energy
Often waste.Inventor is prepared for receiving the carbon molecular sieve of microchannel using waste and old aromatic polyamide reverse osmosis membrane first
Film.
The content of the invention:
A kind of low cost, simple production process are provided, are easy to it is an object of the invention to overcome the shortcomings of above-mentioned prior art
The industrialized method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane, its carbon molecular sieve membrance prepared machinery
Intensity is high, pore structure is flourishing, separating property is good.
The purpose of the present invention can be reached by following measure:
(1) cleaning and preservation of waste and old aromatic polyamide reverse osmosis membrane:By waste and old aromatic polyamide reverse osmosis membrane using super
Method for acoustic cleans, and washes away impurity such as incrustation scale, microorganism etc. of its surface adhesion, then that washed waste and old aromatic polyamide is anti-
Permeable membrane dries in the shade at normal temperatures, is placed in preserving at least 24 hours between two pieces of graphite cakes, flattens.
(2) pore size control agent is put into blender with adhesive under normal temperature to be well mixed, adhesive then requires stronger
Cohesive force and a certain degree of plasticity, the preferably macromolecule such as epoxide-resin glue, polyester resin glue, polysilane base resin glue
For polymer as adhesive, the addition of adhesive is preferably the 85%~99% of mixture gross mass, and pore size control agent is preferably
Zeolite, nano silicon, nano titanium oxide, one or more kinds of mixtures of magnetic iron oxide, by adhesive and
The mixture uniform ground of pore size control agent is coated in from a piece of waste and old aromatic polyamide reverse osmosis membrane taken out between graphite cake
Surface, it is viscous in the above from another waste and old aromatic polyamide reverse osmosis membrane is taken out between graphite cake;Again by two panels bonding
Waste and old aromatic polyamide reverse osmosis membrane is put into seamless molding machine, and control briquetting pressure makes between 0.5~1.0 Mpa
The waste and old aromatic polyamide reverse osmosis membrane of two panels holds tightly together, and it is small to allow it to dry 10 at 60 DEG C in vacuum drying chamber
When.
(3)Bonding, dried waste and old aromatic polyamide reverse osmosis membrane are put into retort, in inert gas shielding
Under charing process is carried out with certain heating rate after just prepare required carbon molecular sieve membrance.Preferably, wherein inert gas
From the one of which of nitrogen, argon gas, heating rate general control in 1~5 DEG C/min, charing final temperature is ordinarily selected to 400~
900 DEG C, and 60~240min of constant temperature at this temperature.
The present invention can produce following good effect compared with the prior art:Applicant is by largely investigating and experiment is ground
Study carefully, the carbon molecular sieve membrance with high value is prepared using waste and old aromatic polyamide reverse osmosis membrane, it has the following advantages that:
(1) carbon molecular sieve membrance that waste and old aromatic polyamide reverse osmosis membrane prepared for persursor material not only production cost is used
It is low, waste and old aromatic polyamide reverse osmosis membrane can be effectively utilized, but also there is higher porosity and flux, pore structure is equal
Even, high mechanical strength.
(2) average pore size of carbon molecular sieve membrance and pore-size distribution are easily controllable.The present invention by change pore size control agent and
Species, addition and the carbonization condition of adhesive can prepare the carbon molecular sieve membrance for different separation requirements.
(3) the carbon molecular sieve membrane porosity prepared is high, and mechanical strength is big, and the smooth zero defect in surface.
Embodiment:
The embodiment of the present invention is elaborated below:
Embodiment 1:
The waste and old aromatic polyamide reverse osmosis membrane of two panels is cleaned by ultrasonic, the impurity of its surface adhesion is washed away, dries in the shade at normal temperatures,
It is positioned between two pieces of graphite cakes and preserves 48 hours, flattens.Weigh 99g polysilane resins respectively and 1g MCM41 zeolites be put into it is mixed
It is well mixed in glassware, by being coated in from being taken out between graphite cake for the mixture uniform ground of polysilane resins and MCM41 zeolites
The surface of a piece of waste and old aromatic polyamide reverse osmosis membrane, from taking out another waste and old aromatic polyamide counter-infiltration between graphite cake
Film is viscous in the above;The waste and old aromatic polyamide reverse osmosis membrane that two panels bonds is put into seamless molding machine again, controlled into
Type pressure makes the waste and old aromatic polyamide reverse osmosis membrane of two panels hold tightly together, and allow it being dried in vacuo in 0.8 MPa
After being dried 10 hours at 60 DEG C in case, it is put into retort, under argon gas protection, 400 DEG C is risen to 1 DEG C/min heating rate
And constant temperature 240min, treat that it is cooled to less than 50 DEG C and can taken out.By test, the average pore size of carbon molecular sieve membrance is 2.0-
3.0nm, porosity 72%.It is 86% to the rejection of disperse dyes under 0.1-0.5Mpa at 20 DEG C.
Embodiment 2:
The waste and old aromatic polyamide reverse osmosis membrane of two panels is cleaned by ultrasonic, the impurity of its surface adhesion is washed away, dries in the shade at normal temperatures,
It is positioned between two pieces of graphite cakes and preserves 48 hours, flattens.90 g epoxide-resin glues and 10 g nano silicons are weighed respectively
It is put into blender and is well mixed, by is coated in from graphite cake for the mixture uniform ground of epoxide-resin glue and nano silicon
Between the surface of a piece of waste and old aromatic polyamide reverse osmosis membrane taken out, from taking out another waste and old aromatic series polyamides between graphite cake
Amine reverse osmosis membrane is viscous in the above;The waste and old aromatic polyamide reverse osmosis membrane that two panels bonds is put into seamless molding machine again
Interior, control briquetting pressure makes the waste and old aromatic polyamide reverse osmosis membrane of two panels hold tightly together in 0.5MPa, and allow its
Dry 10 hours, be put into retort at 60 DEG C in vacuum drying chamber, under argon gas protection, with 2 DEG C/min heating rate liter
To 700 DEG C and the min of constant temperature 120, treat that it is cooled to less than 50 DEG C and can taken out.By test, carbon molecular sieve membrance is averaged
Aperture is 1.0-3.0 nm, porosity 78%.Rejection to disperse dyes under 20 DEG C, 0.1-0.5 Mpa is 90%.
Embodiment 3:
The waste and old aromatic polyamide reverse osmosis membrane of two panels is cleaned by ultrasonic, the impurity of its surface adhesion is washed away, dries in the shade at normal temperatures,
It is positioned between two pieces of graphite cakes and preserves 24 hours, flattens.85g polyester resin glue and 5g ZSM5 zeolites, 5g nanometers are weighed respectively
Titanium dioxide, 5g magnetic iron oxides are put into blender and are well mixed, by polyester resin glue and ZSM5 zeolites and nanometer titanium dioxide
The mixture uniform ground of titanium and magnetic iron oxide is coated in from a piece of waste and old aromatic polyamide reverse osmosis taken out between graphite cake
The surface of permeable membrane, it is viscous in the above from another waste and old aromatic polyamide reverse osmosis membrane is taken out between graphite cake;Two panels is glued again
The waste and old aromatic polyamide reverse osmosis membrane closed is put into seamless molding machine, and control briquetting pressure makes two panels waste and old in 1MPa
Aromatic polyamide reverse osmosis membrane holds tightly together, and allows it to be dried 10 hours at 60 DEG C in vacuum drying chamber, is put into
In retort, under nitrogen protection, 900 DEG C and constant temperature 60min are risen to 5 DEG C/min heating rate, treats that it is cooled to 50 DEG C
It can take out below.By test, the average pore size of carbon molecular sieve membrance is 0.5-2.0nm, porosity 85%.At 20 DEG C,
It is 95% to the rejection of disperse dyes under 0.1-0.5Mpa.
Embodiment 4:
The waste and old aromatic polyamide reverse osmosis membrane of two panels is cleaned by ultrasonic, the impurity of its surface adhesion is washed away, dries in the shade at normal temperatures,
It is positioned between two pieces of graphite cakes and preserves 48 hours, flattens.92 g epoxide-resin glues are weighed respectively and 8 g nano titanium oxides are put
Enter in blender and be well mixed, by being coated in between graphite cake for the mixture uniform ground of epoxide-resin glue and nano titanium oxide
The surface of a piece of waste and old aromatic polyamide reverse osmosis membrane taken out, from taking out another waste and old aromatic polyamide between graphite cake
Reverse osmosis membrane is viscous in the above;The waste and old aromatic polyamide reverse osmosis membrane that two panels bonds is put into seamless molding machine again,
Briquetting pressure is controlled the waste and old aromatic polyamide reverse osmosis membrane of two panels is held tightly together, and allow it true in 0.6MPa
Dry 10 hours, be put into retort at 60 DEG C in empty drying box, under argon gas protection, risen to 3 DEG C/min heating rate
800 DEG C and the min of constant temperature 120, treat that it is cooled to less than 50 DEG C and can taken out.By test, the average hole of carbon molecular sieve membrance
Footpath is 2.0-4.0 nm, porosity 84%.Rejection to disperse dyes under 20 DEG C, 0.1-0.5 Mpa is 85%.
Embodiment 5:
The waste and old aromatic polyamide reverse osmosis membrane of two panels is cleaned by ultrasonic, the impurity of its surface adhesion is washed away, dries in the shade at normal temperatures,
It is positioned between two pieces of graphite cakes and preserves 36 hours, flattens.95 g epoxide-resin glues are weighed respectively and 5 g magnetic iron oxides are put into
It is well mixed in blender, being coated in between graphite cake for mixture uniform ground of epoxide-resin glue and magnetic iron oxide is taken out
A piece of waste and old aromatic polyamide reverse osmosis membrane surface, from taking out another waste and old aromatic polyamide reverse osmosis between graphite cake
Permeable membrane is viscous in the above;The waste and old aromatic polyamide reverse osmosis membrane that two panels bonds is put into seamless molding machine again, controlled
Briquetting pressure makes the waste and old aromatic polyamide reverse osmosis membrane of two panels hold tightly together, and allow it to be done in vacuum in 0.9MPa
Dry 10 hours, be put into retort at 60 DEG C in dry case, under argon gas protection, 850 are risen to 4 DEG C/min heating rate
DEG C and the min of constant temperature 90, treat that it is cooled to less than 50 DEG C and can taken out.By test, the average pore size of carbon molecular sieve membrance is
3.0-4.0 nm, porosity 88%.Rejection to disperse dyes under 20 DEG C, 0.1-0.5 Mpa is 87%.
Embodiment above is only that the preferred embodiment of the present invention is described, and other preferred embodiments are herein
Do not tire out one by one and state, and not the scope of the present invention is defined, on the premise of design spirit of the present invention is not departed from, this area
The various modifications and improvement that ordinary skill technical staff makes to technical scheme, the right that all should fall within the present invention will
In the protection domain for asking book determination.
Claims (6)
- A kind of 1. method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane, it is characterised in that it includes as follows Step:(1) first waste and old aromatic polyamide reverse osmosis membrane is cleaned by ultrasonic, washes away the impurity of its surface adhesion, then will It dries in the shade at normal temperatures, is placed in preserving at least 24 hours between two pieces of graphite cakes, flattens;(2) adhesive and pore size control agent are positioned in blender under normal temperature, make it well mixed;(3) from a piece of waste and old aromatic polyamide reverse osmosis membrane is taken out between graphite cake, by adhesive and the mixing of pore size control agent The surface for being coated in waste and old aromatic polyamide reverse osmosis membrane of thing uniform ground, take another waste and old aromatic polyamide counter-infiltration Film is viscous in the above;The waste and old aromatic polyamide reverse osmosis membrane that two panels bonds is put into seamless molding machine again, controlled into Type pressure makes the waste and old aromatic polyamide reverse osmosis membrane of two panels hold tightly together, and allow it between 0.5~1.0 Mpa Dried 10 hours at 60 DEG C in vacuum drying chamber;(4) bonding, dried waste and old aromatic polyamide reverse osmosis membrane are put into retort, under inert gas shielding Heating charing obtains carbon molecular sieve membrance.
- 2. a kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane according to claim 1, It is characterized in that described waste and old aromatic polyamide reverse osmosis membrane is the waste and old aromatic polyamide reverse osmosis membrane of water purifier.
- 3. a kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane according to claim 1, It is characterized in that the addition of described adhesive is the 85%~99% of the mixture gross mass of adhesive and pore size control agent.
- A kind of 4. side that carbon molecular sieve membrance is prepared with waste and old aromatic polyamide reverse osmosis membrane according to claim 1 or 3 Method, it is characterised in that described adhesive is one kind in epoxide-resin glue, polyester resin glue, polysilane base resin glue.
- A kind of 5. side that carbon molecular sieve membrance is prepared with waste and old aromatic polyamide reverse osmosis membrane according to claim 1 or 3 Method, it is characterised in that described pore size control agent is zeolite, nano silicon, nano titanium oxide, the one of magnetic iron oxide Kind or more than one mixture.
- 6. a kind of method for preparing carbon molecular sieve membrance with waste and old aromatic polyamide reverse osmosis membrane according to claim 1, It is characterized in that it is characterized in that being carbonized in described step (4) under inert atmosphere, inert gas is nitrogen or argon gas, and heating is fast Rate is 1~5 DEG C/min, and charing final temperature is 400~900 DEG C, and the min of constant temperature 60~240 at this temperature.
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Application publication date: 20180323 |