CN107349792A - One kind regeneration membrane module and its manufacture method - Google Patents
One kind regeneration membrane module and its manufacture method Download PDFInfo
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- CN107349792A CN107349792A CN201610305873.2A CN201610305873A CN107349792A CN 107349792 A CN107349792 A CN 107349792A CN 201610305873 A CN201610305873 A CN 201610305873A CN 107349792 A CN107349792 A CN 107349792A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D65/00—Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
- B01D65/02—Membrane cleaning or sterilisation ; Membrane regeneration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/04—Backflushing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/162—Use of acids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2321/00—Details relating to membrane cleaning, regeneration, sterilization or to the prevention of fouling
- B01D2321/16—Use of chemical agents
- B01D2321/164—Use of bases
Abstract
The present invention relates to one kind to regenerate membrane module, the regeneration membrane module includes former membrane module and the cross-linked layer on the surface for investing former membrane module, the cross-linked layer is that cross-linking modified obtain is carried out by siloxanes pre-polymerization liquid to the surface of the former membrane module, the siloxanes pre-polymerization liquid is made up of performed polymer and inert organic solvents, and the performed polymer is the copolymer that more alkoxy silanes are polymerize to obtain with functional monomer.The invention further relates to a kind of preparation method for regenerating membrane module.
Description
Technical field
The present invention relates to membrane module application field, more particularly to a kind of membrane module by surface-crosslinked regeneration and its
Preparation method.
Background technology
Since early 20th century, membrane separation technique is developed rapidly.Divide because membrane separation technique both had
From, concentration, purifying and refined function, have again efficiently, high accuracy, process are simple, easily controllable etc. have
Point, thus it has been obtained widely in fields such as food, medicine, biology, environmental protection, chemical industry, water process
Using.Core component in membrane separation technique is membrane module.Nowadays, on the market membrane separation plant on sale and
Corresponding membrane module species is various.
However, various membrane modules, such as organic film, inoranic membrane, reverse osmosis membrane, NF membrane, milipore filter, micro-
Filter membrane etc., exist because energy resource consumption in UF membrane running caused by the interface pollution of film and cost increase this
One problem.At present in use, it usually needs regularly membrane module is cleaned, to maintain film normally to divide
From performance and flux.But with the extension of disengaging time, membrane module can be gradually because pollutant accumulation and bacterium
Bred etc. microbial growth and cause performance degradation or even failure.Thus, membrane module need to be changed.Mesh
Before, the membrane module changed is all taken as industrial refuse or domestic rubbish disposal, and this largely increases
Add the input of operating cost, more bring the pollution of environment.
The content of the invention
In view of this, the present invention provides a kind of regeneration membrane module for solving existing at least one technical problem
And preparation method thereof.
The present invention provides a kind of regeneration membrane module, and the regeneration membrane module includes former membrane module and invests former film
The cross-linked layer on the surface of device, the cross-linked layer are the surface by siloxanes pre-polymerization liquid to the former membrane module
Carry out cross-linking modified and obtain, the siloxanes pre-polymerization liquid is made up of performed polymer and inert organic solvents, described
The copolymer that performed polymer is polymerize to obtain for more alkoxy silanes with functional monomer, more alkoxyl silicones
Alkane be vinyltrimethoxy silane, VTES, methyl vinyl diethoxysilane,
At least one of methacryloxypropyl trimethyl silane, the functional monomer are methacrylic acid
Hydroxyl ethyl ester, hydroxy propyl methacrylate, dimethylaminoethyl acrylate methyl ammonia ethyl ester, acrylic acid, N- (3- dimethylaminos
Propyl group) Methacrylamide, polyethylene glycol methacrylate-styrene polymer, methyl methacrylate, acrylamide,
At least one of NVP.
Preferably, the ratio that the quality of the cross-linked layer accounts for the quality of the regeneration membrane module is 3%~25%,
The thickness of the cross-linked layer is 1 nanometer~100 nanometers.
Preferably, the former membrane module is at least one of tubular membrane, curtain type membrane, pillar film, Flat Membrane.
Preferably, the inert organic solvents are ethanol, triethyl phosphate, DMF, N, N-
Dimethyl acetamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, at least one of trimethyl phosphate, it is described
The ratio of performed polymer and the inert organic solvents is (2g~50g):100mL.
The present invention also provides a kind of preparation method of above-mentioned regeneration membrane module, and it comprises the following steps:
(1) a siloxanes pre-polymerization liquid is provided, and the siloxanes pre-polymerization liquid is diluted by a diluent;
(2) impregnation is carried out in the siloxanes pre-polymerization liquid that former membrane module is placed in after dilution;And
(3) the former membrane module after impregnation is subjected to precrosslink reaction, obtains the regeneration membrane module.
Preferably, the preparation method of siloxanes pre-polymerization liquid is as follows described in step (1):First by more alkoxy silanes,
Functional monomer and initiator are added in inert organic solvents, obtain a mixture;Then the mixture is added
Heat simultaneously carries out polymerisation under an inert atmosphere, obtains the siloxanes pre-polymerization liquid.
Preferably, the initiator be dibenzoyl peroxide, dialkyl peroxide, azo-bis-isobutyl cyanide,
At least one of the different cyanogen in heptan of azo two, azo-bis-iso-dimethyl, azo isobutyl cyano group formamide, institute
The ratio for stating more alkoxy silanes, functional monomer, initiator and inert organic solvents is:
(1g~25g):(1g~25g):(0.05g~0.5g):100mL, the reaction temperature of the polymerisation is 50 degrees Celsius
~100 degrees Celsius, the reaction time is 2 hours~48 hours.
Preferably, diluent described in step (1) is water and ethanol blend, the siloxanes pre-polymerization liquid with it is dilute
The volume ratio for releasing agent is 1:4~4:1.
Preferably, former membrane module described in step (2) also includes a pair of former membrane modules before impregnation
The step of carrying out cleaning treatment.
Preferably, the catalyst of step (3) precrosslink reaction be hydrochloric acid, sulfuric acid, acetic acid, citric acid,
Phosphoric acid, sodium hydroxide, potassium hydroxide, sodium citrate, sodium acid carbonate, ammonium chloride, at least the one of ammonium sulfate
Kind, the reaction temperature of the precrosslink reaction is 40 degrees Celsius~100 degrees Celsius, and the reaction time is 4 hours~48
Hour.
Compared with prior art, advantages of the present invention is as follows:First, by the siloxanes pre-polymerization liquid to institute
State former membrane module surface carry out it is cross-linking modified and former membrane module surface formed cross-linked layer, the cross-linked layer with
The surface of the former membrane module is tightly tangled and the structure that is combined as a whole, the surface property of the regeneration membrane module
It is stable, and surface-crosslinked modifying process does not destroy the original appearance structure in film surface, also not injury of primary membrane module
Physical and mechanical properties.The obtained regeneration membrane module can recover original performance and come into operation again, significantly
Reduce operating cost, it may have it is green the characteristics of.Second, the cross-linked layer is to pass through feature list
Body is formed with surface-crosslinked modification of the performed polymer that more alkoxy silanes polymerize to obtain to former membrane module, thus
Can be by the independent assortment of functional monomer, and functional performed polymer can be formed, so that the regeneration membrane
The surface of device has the new function such as hydrophily, antipollution and antibacterial.
The preparation method of the regeneration membrane module has the advantages of condition is relatively gentleer, technique is simple, can be achieved
To the batch regeneration of useless, old membrane module or on-line regeneration, the multiple regeneration to waste and old membrane module can be also realized,
It is suitable for scale industrial production.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method of regeneration membrane module of the present invention.
Embodiment
Regeneration membrane module provided by the invention and preparation method thereof will be described further below.
The present invention provides a kind of preparation method for regenerating membrane module, and it includes following steps:
S1, there is provided a siloxanes pre-polymerization liquid, and the siloxanes pre-polymerization liquid is diluted by a diluent;
S2, by former membrane module be placed in dilution after siloxanes pre-polymerization liquid in carry out impregnation;And
S3, the former membrane module after impregnation is subjected to precrosslink reaction, obtains the regeneration membrane module.
In step sl, the diluent is used to the siloxanes pre-polymerization liquid being diluted.The diluent
For water and ethanol blend.The mixed proportion of the water and ethanol is unlimited.The siloxanes pre-polymerization liquid and dilution
The volume ratio of agent is 1:4~4:1.
The preparation method of the siloxanes pre-polymerization liquid is as follows:
S11, more alkoxy silanes, functional monomer and initiator are added in inert organic solvents, obtain one
Mixture;
S12, the mixture is heated and carries out polymerisation under an inert atmosphere, obtains the siloxanes pre-polymerization
Liquid.
In step s 11, the function that the functional monomer can be modified according to surface needs and selected, specifically
Be the monomer containing unsaturated carbon-carbon double bond (C=C).More alkoxy silanes are containing unsaturated carbon-carbon double bond
(C=C) more alkoxy silanes.The effect of more alkoxy silanes and functional monomer in the initiator
Lower generation polymerisation obtains performed polymer.Specifically, more alkoxy silanes are vinyl trimethoxy silicon
Alkane, VTES, methyl vinyl diethoxysilane, methacryloxypropyl three
At least one of methyl-monosilane.The functional monomer is hydroxyethyl methacrylate, hydroxyethyl methacrylate
Propyl ester, dimethylaminoethyl acrylate methyl ammonia ethyl ester, acrylic acid, N- (3- dimethylamino-propyls) Methacrylamide,
In polyethylene glycol methacrylate-styrene polymer, methyl methacrylate, acrylamide, NVP
It is at least one.
The initiator act as initiated polymerization.The initiator is organic peroxide initiator
And/or azo-initiator.The organic peroxide initiator is dibenzoyl peroxide, dialkyl group mistake
At least one of oxide, the azo-initiator are azo-bis-isobutyl cyanide, the different cyanogen in heptan of azo two, idol
At least one of the isobutyl dimethyl phthalate of nitrogen two, azo isobutyl cyano group formamide.The dosage of the initiator compared with
It is few, can be depending on specific reactant and its dosage.
The mass ratio of more alkoxy silanes and functional monomer is 2:1~1:3, be preferably, 2:1~1:2.
The performed polymer for acting as obtaining of the inert organic solvents preserves in liquid form, isolates moisture
Deng induction, prevent that performed polymer from occurring hydrolytic crosslinking in storage process, and be allowed to be in metastable shape
State, and can preserve for a long time.The inert organic solvents are ethanol, triethyl phosphate, N, N- dimethyl methyls
Acid amides, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), 1-METHYLPYRROLIDONE, trimethyl phosphate are at least
It is a kind of.The dosage of the inert organic solvents according to specific needs depending on, it is however generally that, the inertia is organic
The dosage of solvent is less, to facilitate the needs for preserving and transporting.That is, described more alkoxy silanes with it is described
The ratio of inert organic solvents is:(1g~25g):(80mL~150mL).
Preferably, the ratio of more alkoxy silanes, functional monomer, initiator and inert organic solvents
For:(1g~25g):(1g~25g):(0.05g~0.5g):100mL.
In step s 12, the reaction temperature of the polymerisation is 50 degrees Celsius~100 degrees Celsius, during reaction
Between be 2 hours~48 hours.Preferably, the reaction temperature is 65 degrees Celsius~85 degrees Celsius, during reaction
Between be 8 hours~24 hours.
After reaction terminates, obtained performed polymer and the ratio of the inert organic solvents are (2g~50g):100mL,
Preferably, (5g~30g):100mL.
In step s 2, the purpose of the impregnation is the performed polymer is invested into the former membrane device in advance
The surface of part.The time of the impregnation is 0.5 hour~48 hours, is preferably, 1 hour~12 hours.
The material of the former membrane module is at least one of tubular membrane, curtain type membrane, pillar film, Flat Membrane.
The former membrane module also includes the step that a pair of former membrane modules carry out cleaning treatment before impregnation
Suddenly.The cleaning treatment is specially:By the former membrane module carry out successively alkali cleaning, pickling, redox,
The cleaning processes such as backwash are to obtain clean former membrane module after removing pollutant.
In step s3, the former membrane module after impregnation can be moved into the solution containing catalyst and carried out
Precrosslink is reacted.Solvent in the solution containing catalyst is water.The catalyst be hydrochloric acid, sulfuric acid,
Acetic acid, citric acid, phosphoric acid, sodium hydroxide, potassium hydroxide, sodium citrate, sodium acid carbonate, ammonium chloride,
At least one of ammonium sulfate.The concentration of the catalyst is 0mol/L~1mol/L, is preferably
0.01mol/L~0.5mol/L.When the concentration of the catalyst is 0, that is, referring to the precrosslink reaction can be direct
Carried out in water, and without adding catalyst.When being not added with catalyst, the environment of reaction is proposed with deionization
Water.The reaction temperature of the precrosslink reaction is 40 degrees Celsius~100 degrees Celsius, and the reaction time is 4 hours~48
Hour.Preferably, the reaction temperature of the precrosslink reaction is 50 degrees Celsius~80 degrees Celsius, the reaction time
For 8 hours~24 hours.
The present invention also provides a kind of regeneration membrane module being prepared using the above method.The regeneration membrane module
Cross-linked layer including former membrane module and the surface for investing former membrane module, the cross-linked layer are pre- by siloxanes
Poly- liquid is carried out cross-linking modified and obtained to the surface of the former membrane module.
The siloxanes pre-polymerization liquid is made up of performed polymer and inert organic solvents, and the performed polymer is more alkoxies
Silane is polymerize obtained copolymer with functional monomer.
The ratio that the quality of the cross-linked layer accounts for the quality of the regeneration membrane module is 3%~25%, the crosslinking
The thickness of layer is 1 nanometer~100 nanometers.Preferably, the quality of the cross-linked layer accounts for the regeneration membrane module
The ratio of quality is 3%~15%, and the thickness of the cross-linked layer is 10 nanometers~50 nanometers.
Compared with prior art, advantages of the present invention is as follows:First, by the siloxanes pre-polymerization liquid to institute
State former membrane module surface carry out it is cross-linking modified and former membrane module surface formed cross-linked layer, the cross-linked layer with
The surface of the former membrane module is tightly tangled and the structure that is combined as a whole, the surface property of the regeneration membrane module
It is stable, and surface-crosslinked modifying process does not destroy the original appearance structure in film surface, also not injury of primary membrane module
Physical and mechanical properties.The obtained regeneration membrane module can recover original performance and come into operation again, significantly
Reduce operating cost, it may have it is green the characteristics of.Second, the cross-linked layer is to pass through feature list
Body is formed with surface-crosslinked modification of the performed polymer that more alkoxy silanes polymerize to obtain to former membrane module, thus
Can be by the independent assortment of functional monomer, and functional performed polymer can be formed, so that the regeneration membrane
The surface of device has the new function such as hydrophily, antipollution and antibacterial.
The preparation method of the regeneration membrane module has the advantages of condition is relatively gentleer, technique is simple, can be achieved
To the batch regeneration of useless, old membrane module or on-line regeneration, the multiple regeneration to waste and old membrane module can be also realized,
It is suitable for scale industrial production.
Hereinafter, will be further to regeneration membrane module of the present invention and preparation method thereof in conjunction with specific embodiments
Explanation.
Embodiment 1
(1) by the mistake of 3g hydroxyethyl methacrylate, 2g vinyltrimethoxy silane and 0.06g
BP is added sequentially in 100mL absolute ethyl alcohol, is passed through industrial nitrogen, and at normal temperatures
200r/min mechanical agitations 20min.Then open heating and gradually rise temperature to 65 DEG C, in Industrial Nitrogen atmosphere
In enclosing, 200r/min mechanic whirl-nett reactions 36 hours.Heating is closed, is obtained after abundant cooling hydrophilic
The pre-polymerization liquid of hydroxyethyl methacrylate/vinyltrimethoxy silane copolymer.It is pre- in obtained 100mL again
40mL deionized waters, the pre-polymerization liquid after being diluted are added in poly- liquid.
(2) the tubular type membrane cartridge for changing household water filter, pickling is first carried out, then is done through backwash
Net filter core.
(3) by the tubular type membrane cartridge after the pre-polymerization liquid injection cleaning after enough dilutions, inlet and outlet are sealed, and it is quiet
Put 2 hours.
(4) the pre-polymerization liquid after the dilution in filter core to be poured out, and injects pure water, 60 DEG C of constant temperature stand 8 hours,
Obtain regenerating household water filter tubular type membrane cartridge.
After tested, the regeneration household water filter is recovered as before with the water flux and cutoff performance of tubular type membrane cartridge.
Embodiment 2
(1) by the idol of 4g NVP, 3g VTES and 0.1g
The different cyanogen in heptan of nitrogen two is added sequentially in 100mL triethyl phosphate, is passed through high pure nitrogen, and at normal temperatures
250r/min mechanical agitations 30min.Then open heating and gradually rise temperature to 80 DEG C, in Industrial Nitrogen atmosphere
In enclosing, 250r/min mechanic whirl-nett reactions 24 hours.Heating is closed, is obtained after abundant cooling hydrophilic
NVP/VTES copolymer pre-polymerization liquid.In the 100mL pre-polymerization liquid of gained
Middle addition 100mL 60% ethanol water, the pre-polymerization liquid after being diluted.
(2) the Kynoar curtain type membrane that will be discarded after pollution, alkali cleaning, pickling and hypochlorous acid are first carried out successively
Sodium aoxidizes, then obtains clean curtain type membrane through backwash.
(3) curtain type membrane after cleaning is soaked into the pre-polymerization liquid after enough dilutions, and stands 3 hours;
(4) curtain type membrane is taken out, be soaked into the aqueous hydrochloric acid solution that enough pH are 5,65 DEG C stand 20 hours,
Obtain regenerating Kynoar curtain type membrane.
After tested, the water flux of the regeneration Kynoar curtain type membrane and cutoff performance recover as before.
Embodiment 3
(1) by 6g hydroxy propyl methacrylate, 5g N- polyethylene glycol methacrylate-styrene polymers, 5g first
Base methylvinyldiethoxysilane/3g VTES and 0.2g azo isobutyl cyano group formamide
100mL dimethyl sulfoxide (DMSO) is added sequentially to, is passed through nitrogen, and 200r/min mechanical agitations at normal temperatures
60min.Then open heating and gradually rise temperature to 100 DEG C, in ordinary nitrogen atmosphere, 200r/min machines
Tool stirring reaction 10 hours.Heating is closed, the poly- second two of hydroxy propyl methacrylate/N- is obtained after abundant cooling
The pre-polymerization of alcohol methacrylate/methyl vinyl diethoxysilane/VTES copolymer
Liquid.60mL 35% ethanol water is added in the 100mL pre-polymerization liquid of gained, it is pre- after being diluted
Poly- liquid.
(2) the polysulfones Flat Membrane that will be discarded after pollution, alkali cleaning and pickling are first carried out successively, then obtained through backwash
Clean Flat Membrane.
(3) Flat Membrane after cleaning is soaked into the pre-polymerization liquid after enough dilutions, and stands 2.5 hours.
(4) Flat Membrane is taken out, be soaked into the sodium hydrate aqueous solution that enough pH are 9,70 DEG C stand 24
Hour, that is, obtain regenerating polysulfones Flat Membrane.
After tested, the water flux of the regeneration polysulfones Flat Membrane and cutoff performance recover as before.Meanwhile test knot
Fruit shows that the anti-protein contamination of the regeneration polysulfones Flat Membrane is better than the Flat Membrane of new production.
Embodiment 4
(1) by the N- polyethylene glycol first of 8g N- (3- dimethylamino-propyls) Methacrylamide, 4g
Base acrylate, 4g hydroxyethyl methacrylate, 8g vinyltrimethoxy silane and 0.25g mistake
BP is added sequentially in 100mL absolute ethyl alcohol, is passed through nitrogen, and 200r/min at normal temperatures
Mechanical agitation 60min.Then open heating and gradually rise temperature to 65 DEG C, in ordinary nitrogen atmosphere,
200r/min mechanic whirl-nett reactions 36 hours.Heating is closed, N- (3- dimethylaminos are obtained after abundant cooling
Propyl group) Methacrylamide/N- polyethylene glycol methacrylate-styrene polymers/hydroxyethyl methacrylate/vinyl trimethoxy
The pre-polymerization liquid of base silane copolymer.75% ethanol that 30mL is added in the 100mL pre-polymerization liquid of gained is water-soluble
Liquid, the pre-polymerization liquid after being diluted.
(2) to the pillar film after performance degradation in separation running, online alkali cleaning, pickling are first carried out successively
And liquor natrii hypochloritis's washing, then remove pillar film surface adhesion pollutant through backwash.
(3) by the pre-polymerization liquid online injection pillar film after enough dilutions, circulate 1.5 hours.
(4) the pre-polymerization liquid after dilution to be discharged, is replaced by the aqueous acetic acid that pH is 5, solution temperature is 60 DEG C,
Circulation is replaced by deionized water rinsing 30 minutes after 20 hours, obtains regenerating pillar film.
Through on-line testing, the water flux and cutoff performance of the regeneration pillar film recover as before.Meanwhile identical
Separate under service condition, the performance degradation cycle of the regeneration pillar film is grown compared with the pillar film of new production.This explanation,
After regeneration treatment, the hydrophilicity of pillar film is restored, and antifouling property is improved.
The explanation of above example is only intended to help the method and its core concept for understanding the present invention.It should refer to
Go out, for those skilled in the art, under the premise without departing from the principles of the invention, also
Some improvement and modification can be carried out to the present invention, these are improved and modification also falls into the claims in the present invention
In protection domain.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field is realized or use this
Invention.A variety of modifications to these embodiments will be apparent for those skilled in the art,
Generic principles defined herein can without departing from the spirit or scope of the present invention, other
Realized in embodiment.Therefore, the present invention is not intended to be limited to the embodiments shown herein, but will
Meet the most wide scope consistent with principles disclosed herein and features of novelty.
Claims (10)
1. one kind regeneration membrane module, it is characterised in that the regeneration membrane module includes former membrane module and invested
The cross-linked layer on the surface of former membrane module, the cross-linked layer are to the former membrane module by siloxanes pre-polymerization liquid
Surface carries out cross-linking modified and obtained, and the siloxanes pre-polymerization liquid is made up of performed polymer and inert organic solvents,
The copolymer that the performed polymer is polymerize to obtain for more alkoxy silanes with functional monomer, more alcoxyls
Base silane is vinyltrimethoxy silane, VTES, methyl ethylene diethoxy silicon
At least one of alkane, methacryloxypropyl trimethyl silane, the functional monomer are methyl-prop
Olefin(e) acid hydroxyl ethyl ester, hydroxy propyl methacrylate, dimethylaminoethyl acrylate methyl ammonia ethyl ester, acrylic acid, N- (3- diformazans
Aminopropyl) Methacrylamide, polyethylene glycol methacrylate-styrene polymer, methyl methacrylate, acrylamide,
At least one of NVP.
2. regeneration membrane module as claimed in claim 1, it is characterised in that the quality of the cross-linked layer accounts for institute
The ratio for stating the quality of regeneration membrane module is 3%~25%, and the thickness of the cross-linked layer is 1 nanometer~100 nanometers.
3. as claimed in claim 1 regeneration membrane module, it is characterised in that the former membrane module be tubular membrane,
At least one of curtain type membrane, pillar film, Flat Membrane.
4. regeneration membrane module as claimed in claim 1, it is characterised in that the inert organic solvents are second
Alcohol, triethyl phosphate, N,N-dimethylformamide, DMAC N,N' dimethyl acetamide, dimethyl sulfoxide (DMSO), N- first
The ratio of at least one of base pyrrolidones, trimethyl phosphate, the performed polymer and the inert organic solvents
For (2g~50g):100mL.
5. a kind of preparation method that membrane module is regenerated such as any one of Claims 1 to 4, it comprises the following steps:
(1) a siloxanes pre-polymerization liquid is provided, and the siloxanes pre-polymerization liquid is diluted by a diluent;
(2) impregnation is carried out in the siloxanes pre-polymerization liquid that former membrane module is placed in after dilution;And
(3) the former membrane module after impregnation is subjected to precrosslink reaction, obtains the regeneration membrane module.
6. the preparation method of regeneration membrane module as claimed in claim 5, it is characterised in that institute in step (1)
The preparation method for stating siloxanes pre-polymerization liquid is as follows:First more alkoxy silanes, functional monomer and initiator are added
Enter in inert organic solvents, obtain a mixture;Then the mixture is heated and carried out under an inert atmosphere
Polymerisation, obtain the siloxanes pre-polymerization liquid.
7. the preparation method of regeneration membrane module as claimed in claim 6, it is characterised in that the initiator
For dibenzoyl peroxide, dialkyl peroxide, azo-bis-isobutyl cyanide, the different cyanogen in heptan of azo two, azo two
At least one of isobutyl dimethyl phthalate, azo isobutyl cyano group formamide, more alkoxy silanes, function
The ratio of property monomer, initiator and inert organic solvents is:
(1g~25g):(1g~25g):(0.05g~0.5g):100mL, the reaction temperature of the polymerisation is 50 degrees Celsius
~100 degrees Celsius, the reaction time is 2 hours~48 hours.
8. the preparation method of regeneration membrane module as claimed in claim 5, it is characterised in that institute in step (1)
It is water and ethanol blend to state diluent, and the volume ratio of the siloxanes pre-polymerization liquid and diluent is 1:4~4:1.
9. the preparation method of regeneration membrane module as claimed in claim 5, it is characterised in that institute in step (2)
State former membrane module also includes the step of a pair of former membrane modules carry out cleaning treatment before impregnation.
10. the preparation method of regeneration membrane module as claimed in claim 5, it is characterised in that step (3) institute
The catalyst for stating precrosslink reaction is hydrochloric acid, sulfuric acid, acetic acid, citric acid, phosphoric acid, sodium hydroxide, hydrogen-oxygen
Change potassium, sodium citrate, sodium acid carbonate, ammonium chloride, at least one of ammonium sulfate, the precrosslink reaction
Reaction temperature is 40 degrees Celsius~100 degrees Celsius, and the reaction time is 4 hours~48 hours.
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CN1646607A (en) * | 2002-04-11 | 2005-07-27 | 瓦克聚合系统两合公司 | Organofunctional silicone copolymers and the saponification products thereof |
CN102863647A (en) * | 2012-09-19 | 2013-01-09 | 合肥工业大学 | Preparation method of organic-inorganic hybrid ionic membrane |
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