CN106268374B - A kind of solvent-resistant compound nanofiltration membrane and preparation method - Google Patents
A kind of solvent-resistant compound nanofiltration membrane and preparation method Download PDFInfo
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- CN106268374B CN106268374B CN201510279540.2A CN201510279540A CN106268374B CN 106268374 B CN106268374 B CN 106268374B CN 201510279540 A CN201510279540 A CN 201510279540A CN 106268374 B CN106268374 B CN 106268374B
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Abstract
The invention discloses a kind of solvent-resistant compound nanofiltration membrane and preparation method, preparation method is：(1) polyetherimide and organic solvent are mixed, at 35-80 DEG C, stirring, then at 6-25 DEG C, standing and defoaming, casting solution is made, scrapes casting solution in non-woven fabrics, places in air, deionized water is impregnated, taking-up blots surface moisture with filter paper, obtains basement membrane, claims the one side for scraping casting solution of non-woven fabrics to the faces A；(2) faces A of basement membrane are soaked in ethylenediamine methanol solution, take out, is washed with deionized, the film after being crosslinked；(3) faces A of the film after crosslinking are immersed in lignin sulfonic acid aqueous ammonium, taken out, then the faces A are immersed in pyromellitic trimethylsilyl chloride hexane solution, taken out, dry, obtain a kind of solvent-resistant compound nanofiltration membrane.The present invention is at low cost, and method is simple, is swift in response；The composite nanometer filtering film of acquisition possesses higher separation selectivity and solvent tolerance.
Description
Technical field
The present invention relates to a kind of solvent-resistant compound nanofiltration membrane and preparation methods.
Background technology
Nanofiltration is the novel membrane separation technique risen in recent ten years.Nanofiltration belongs to pressure-actuated membrane process,
In performance between reverse osmosis between ultrafiltration membrane, molecular cut off is generally in 200~1000 ranges.Have to divalent and high price salt
Higher removal efficiency is hundreds of organic matter and divalent, high price inorganic salts etc. particularly suitable for separation molecular weight.
NF membrane can formally be divided into anisotropic membrane and homogeneous membrane.Wherein anisotropic membrane is by ultra-thin dense layer surface and more
The support substrate in hole forms.Interfacial polymerization is at present using most, the most effective method for preparing nanofiltration solvent resistant film.The party
Method general process is：It is first absorbed dissolved with a kind of monomer or the aqueous phase solution of prepolymer with porous basement membrane, it is extra to take the film out exclusion
It after solution, then contacts with the oil phase (such as hexamethylene) dissolved with another monomer or prepolymer, liquid-liquid interface reaction is carried out, in two phase boundaries
Film is formed at face.
In recent years, as the application of NF membrane, the stalling characteristic of nanofiltration are further excavated, NF membrane is not only limited to
In the separation of aqueous phase system, is more and more used as the separation system of medium needs using organic solvent and have solvent resistance
The purification of polar molecule, the recycling of polar solvent in NF membrane, such as chemical industry, biology, field of medicaments.Currently, being commercialized
Nanofiltration membrane material mainly have polyamide (PA), polyvinyl alcohol (PVA), sulfonated polysulfone (SPS), sulfonated polyether sulfone (SPES), vinegar
Acid cellulose (CA) and its derivative etc..[Yao Guoying, nanofiltration membrane material and its application Shanghai Institute Of Technology journal:It is natural
Science version, 2004,3 (4):255-259.] NF membrane that is gone out by these material preparations can show ten in water solution system
Divide outstanding separating property, but swelling or dissolution phenomena can then occur in organic system, the decline of separating property is caused [to open
New sunshine, Yuan Qipeng, progress and its application membrane science and technology of the nanofiltration in organic phase separation, 2005,25:53-
57]。
How effectively ammonium lignosulphonate has the characteristics that amount of storage is big, inexpensive as paper industry principal by product, profit
It is always scientific research personnel's focus of attention with lignin sulfonate resource.
Invention content
The purpose of the present invention is overcome the deficiencies of the prior art and provide a kind of to have selectivity good, solvent resistance strong
Solvent-resistant compound nanofiltration membrane.
Second object of the present invention is to provide that a kind of solvent resistant for the byproduct that can efficiently use paper industry is compound to be received
Filter membrane and preparation method.
Technical scheme of the present invention is summarized as follows：
A kind of preparation method of solvent-resistant compound nanofiltration membrane, includes the following steps：
(1) polyetherimide and organic solvent are mixed, makes the mass concentration of polyetherimide-organic solvent solution be
15%-40% is stirred 3-8 hours, then at 6-25 DEG C of temperature, casting solution is made in standing and defoaming 3-24 hours at 35-80 DEG C,
By 600cm2:The ratio of 12-20g scrapes casting solution on a shiny surface of the non-woven fabrics of at least one shiny surface, in air
Middle placement 5-60 seconds, places into deionized water, impregnates 5-60 minutes, and taking-up blots surface moisture with filter paper, obtains basement membrane, will
The one side for scraping casting solution of non-woven fabrics claims the faces A；
(2) faces A of basement membrane are soaked in the ethylenediamine methanol solution that mass concentration is 0.1%-20%, impregnate 0.5-1
Hour, it takes out, is washed with deionized 2-4 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in 1-2 points of the lignin sulfonic acid aqueous ammonium that mass concentration is 1%-20%
Clock, taking-up blot surface moisture with filter paper, then that the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in quality is dense
Degree is to take out after 30-60 seconds, dry in air, obtain resistance to molten in the pyromellitic trimethylsilyl chloride hexane solution of 1.5%-15%
Agent composite nanometer filtering film.
The preferred 15%-30% of mass concentration of polyetherimide-organic solvent solution.
The preferred n,N-dimethylacetamide of organic solvent, N-Methyl pyrrolidone or n,N-Dimethylformamide.
The preferred 1%-10% of mass concentration of lignin sulfonic acid aqueous ammonium.
Solvent-resistant compound nanofiltration membrane prepared by the above method.
The advantage of the invention is that：
1. the present invention using amount of storage big paper industry principal by product ammonium lignosulphonate as interface polymerization reaction object,
Application for lignosulfonates from now in UF membrane industry provides good technical foundation.
2. the method for the present invention is simple for process, it is swift in response.
3. the solvent-resistant compound nanofiltration membrane that the method for the present invention obtains possesses higher separation selectivity and solvent tolerance.
4. will be greatly lowered in current NF membrane preparation process by interface polymerization reaction object of ammonium lignosulphonate
The use of the expensive chemicals such as piperazine, phenylenediamine makes the cost of film preparation decline.
Description of the drawings
Fig. 1 is the cross-section morphology of prepared solvent-resistant compound nanofiltration membrane.
Specific implementation mode
With reference to specific embodiment, the present invention is further illustrated, and the embodiment of the present invention is to make this field
Technical staff better understood when the present invention, but the present invention is not imposed any restrictions.
Swellbility measures：Sample film is cut into the small item of 3 × 1cm, reaches constant weight, electricity consumption after being placed at 110 DEG C dry 4h
Sub- balance weighs the quality of dry film, is denoted as m0, dry film is placed in the conical flask for filling organic solvent, is shaken in 30 DEG C of water-bath
Sample is taken out after swinging 48h, is rapidly blotted sample surfaces with filter paper, with the quality of electronic balance weighing wet film, is denoted as mt.Swelling
Degree S is calculated with following formula：
Embodiment 1
A kind of preparation method of solvent-resistant compound nanofiltration membrane, includes the following steps：
(1) polyetherimide and n,N-dimethylacetamide are mixed, keeps polyetherimide-n,N-dimethylacetamide molten
The mass concentration of liquid is 15%, at 35 DEG C, is stirred 3 hours, then in 15 DEG C of temperature, standing and defoaming 12 hours is made casting solution, presses
600cm2:The ratio of 12g scrapes casting solution on there are one the shiny surface of the non-woven fabrics of shiny surface, places 5 seconds in air, then put
Enter in deionized water, impregnate 10 minutes, taking-up blots surface moisture with filter paper, obtain basement membrane, by the casting solution of scraping of non-woven fabrics
Claim the faces A on one side；
(2) faces A of basement membrane are soaked in the ethylenediamine methanol solution that mass concentration is 0.1%, soaking time 1 hour,
It takes out, is washed with deionized 3 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in the lignin sulfonic acid aqueous ammonium 2 minutes that mass concentration is 2%, taken out
Surface moisture is blotted with filter paper, then the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in mass concentration and are
In 1.5% pyromellitic trimethylsilyl chloride hexane solution, takes out after 40 seconds, dry in air, obtain composite nanometer filtering film.
The cross-section morphology of composite nanometer filtering film is shown in Fig. 1, from figure 1 it appears that the section structure of composite nanometer filtering film is by relatively thin
And fine and close active separating layer is constituted with finger-like pore supporting layer two parts, has the typical unsymmetric structure of NF membrane.
The flux of gained film is 33.7L h-1m-2MPa-1, filted chroma is the cotton seed sugar aqueous solution of 10g/L, and rejection is
92%.
Solvent resistance：Show that solvent resistance, prepared composite nanometer filtering film soak in several solvents using swelling ratio
Bubble tests its swelling ratio after 48 hours, and the swelling ratio in n,N-dimethylacetamide is 1.24, N-, n,N-Dimethylformamide
In swelling ratio be 1.14, the swelling ratio in dimethyl sulfoxide (DMSO) is 1.72, the swelling ratio in tetrahydrofuran is 1.10.
Embodiment 2
A kind of preparation method of solvent-resistant compound nanofiltration membrane, includes the following steps：
(1) polyetherimide and n,N-Dimethylformamide are mixed, keeps polyetherimide-n,N-Dimethylformamide molten
The mass concentration of liquid is 40%, at 80 DEG C, mixing time 8 hours, then in 20 DEG C of temperature, casting film is made in standing and defoaming 5 hours
Liquid, by 600cm2:The ratio of 15g scrapes casting solution on there are one the shiny surface of the non-woven fabrics of shiny surface, places 30 in air
Second, it places into deionized water, impregnates 40 minutes, taking-up blots surface moisture with filter paper, obtains basement membrane, and non-woven fabrics is scraped casting
The one side of film liquid claims the faces A；
(2) faces A of basement membrane are soaked in the ethylenediamine methanol solution that mass concentration is 20%, soaking time 1 hour takes
Go out, is washed with deionized 3 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in the aqueous solution 2 minutes for the ammonium lignosulphonate that mass concentration is 10%,
Taking-up blots surface moisture with filter paper, then the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in mass concentration
In 5% pyromellitic trimethylsilyl chloride hexane solution, to take out after 60 seconds, drying in air, obtain solvent-resistant compound nanofiltration membrane.
Prepared composite nanometer filtering film cross-section morphology is similar to embodiment 1.
The flux of gained film is 15.9L h-1m-2MPa-1, filted chroma is the cotton seed sugar aqueous solution of 10g/L, and rejection is
93%.
Solvent resistance：Show that solvent resistance, prepared composite nanometer filtering film soak in several solvents using swelling ratio
Bubble tests its swelling ratio after 48 hours, and the swelling ratio in n,N-dimethylacetamide is in 1.2, N-, n,N-Dimethylformamide
Swelling ratio be 1.05, the swelling ratio in dimethyl sulfoxide (DMSO) is 1.52, the swelling ratio in tetrahydrofuran is 1.0.
Embodiment 3
A kind of preparation method of solvent-resistant compound nanofiltration membrane, includes the following steps：
(1) polyetherimide and n,N-Dimethylformamide are mixed, keeps polyetherimide-n,N-Dimethylformamide molten
The mass concentration of liquid is 30%, at 35 DEG C, mixing time 4 hours, then in 6 DEG C of temperature, casting film is made in standing and defoaming 24 hours
Liquid, by 600cm2:The ratio of 20g scrapes casting solution on there are one the shiny surface of the non-woven fabrics of shiny surface, places 60 in air
Second, it places into deionized water, impregnates 5 minutes, taking-up blots surface moisture with filter paper, obtains basement membrane, and non-woven fabrics is scraped casting
The one side of film liquid claims the faces A；
(2) faces A of basement membrane are soaked in the ethylenediamine methanol solution that mass concentration is 10%, impregnate 0.5 hour, takes
Go out, is washed with deionized 2 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in the aqueous solution 2 minutes for the ammonium lignosulphonate that mass concentration is 20%,
Taking-up blots surface moisture with filter paper, then the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in mass concentration
In 10% pyromellitic trimethylsilyl chloride hexane solution, to take out after 30 seconds, drying in air, solvent resistant composite nanometer filter is obtained
Film.Prepared composite nanometer filtering film cross-section morphology is similar to embodiment 1.
The flux of gained film is 18.6L h-1m-2MPa-1, filted chroma is the cotton seed sugar aqueous solution of 10g/L, and rejection is
89%.
Solvent resistance：Show that solvent resistance, prepared composite nanometer filtering film soak in several solvents using swelling ratio
Bubble tests its swelling ratio after 48 hours, and the swelling ratio in n,N-dimethylacetamide is 1.47, N-, n,N-Dimethylformamide
In swelling ratio be 1.45, the swelling ratio in dimethyl sulfoxide (DMSO) is 1.82, the swelling ratio in tetrahydrofuran is 0.93.
Embodiment 4
A kind of preparation method of solvent-resistant compound nanofiltration membrane, includes the following steps：
(1) polyetherimide and N-Methyl pyrrolidone are mixed, makes polyetherimide-N-Methyl pyrrolidone solution
Mass concentration is 18%, at 65 DEG C, mixing time 5 hours, then in 25 DEG C of temperature, standing and defoaming 3 hours is made casting solution, presses
600cm2:The ratio of 18g scrapes casting solution on there are two the non-woven fabrics of shiny surface a shiny surface, places 40 in air
Second, it places into deionized water, impregnates 60 minutes, taking-up blots surface moisture with filter paper, obtains basement membrane, and non-woven fabrics is scraped casting
The one side of film liquid claims the faces A；
(2) faces A of basement membrane are soaked in the ethylenediamine methanol solution that mass concentration is 8%, soaking time 1 hour takes
Go out, is washed with deionized 4 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in the aqueous solution 1 minute for the ammonium lignosulphonate that mass concentration is 1%, are taken
Go out and blot surface moisture with filter paper, then the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in mass concentration and are
In 15% pyromellitic trimethylsilyl chloride hexane solution, takes out after 50 seconds, dry in air, obtain solvent-resistant compound nanofiltration membrane.
Prepared composite nanometer filtering film cross-section morphology is similar to embodiment 1.
The flux of gained film is 19.21L h-1m-2MPa-1, filted chroma is the cotton seed sugar aqueous solution of 10g/L, and rejection is
91%.
Solvent resistance：Show that solvent resistance, prepared composite nanometer filtering film soak in several solvents using swelling ratio
Bubble tests its swelling ratio after 48 hours, and the swelling ratio in n,N-dimethylacetamide is 1.89, N-, n,N-Dimethylformamide
In swelling ratio be 2.24, the swelling ratio in dimethyl sulfoxide (DMSO) is 1.92, the swelling ratio in tetrahydrofuran is 1.07.
Claims (5)
1. a kind of preparation method of solvent-resistant compound nanofiltration membrane, it is characterized in that including the following steps：
(1) polyetherimide and organic solvent are mixed, it is 15%- to make the mass concentration of polyetherimide-organic solvent solution
40%, at 35-80 DEG C, stir 3-8 hours, then at 6-25 DEG C of temperature, standing and defoaming 3-24 hours is made casting solution, presses
600cm2:The ratio of 12-20g scrapes casting solution on a shiny surface of the non-woven fabrics of at least one shiny surface, in air
It places 5-60 seconds, places into deionized water, impregnate 5-60 minutes, taking-up blots surface moisture with filter paper, obtains basement membrane, by nothing
The one side for scraping casting solution of woven fabric claims the faces A；
(2) faces A of basement membrane are soaked in the methanol solution for the ethylenediamine that mass concentration is 0.1%-20%, it is small impregnates 0.5-1
When, it takes out, is washed with deionized 2-4 times, the film after being crosslinked；
(3) faces A of the film after crosslinking are immersed in lignin sulfonic acid aqueous ammonium 1-2 minutes that mass concentration is 1%-20%,
Taking-up blots surface moisture with filter paper, then the faces A of the film after the crosslinking for impregnating ammonium lignosulphonate are immersed in mass concentration
In the pyromellitic trimethylsilyl chloride hexane solution of 1.5%-15%, to take out after 30-60 seconds, drying in air, obtain solvent resistant
Composite nanometer filtering film.
2. the preparation method of a kind of solvent-resistant compound nanofiltration membrane according to claim 1, it is characterized in that polyetherimide-has
The mass concentration of solvent solution is 15%-30%.
3. the preparation method of a kind of solvent-resistant compound nanofiltration membrane according to claim 1 or 2, it is characterized in that described organic molten
Agent is n,N-dimethylacetamide, N-Methyl pyrrolidone or n,N-Dimethylformamide.
4. the preparation method of a kind of solvent-resistant compound nanofiltration membrane according to claim 1, it is characterized in that ammonium lignosulphonate
The mass concentration of aqueous solution is 1%-10%.
5. solvent-resistant compound nanofiltration membrane prepared by the method described in one of claim 1-4.
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| CN111437740A (en) * | 2020-03-09 | 2020-07-24 | 哈尔滨工业大学 | Preparation method of sodium lignosulphonate-based high-flux high-interception nanofiltration membrane |
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| CN106890571A (en) * | 2017-03-06 | 2017-06-27 | 江苏凯米膜科技股份有限公司 | A kind of preparation method of organic tubular nanofiltration membrane |
| CN109364759A (en) * | 2018-12-21 | 2019-02-22 | 滁州学院 | A kind of calcium lignosulfonate solvent-resistant compound nanofiltration membrane and preparation method thereof |
| CN109351192B (en) * | 2018-12-21 | 2021-07-20 | 滁州学院 | Anethol solvent-resistant composite nanofiltration membrane and preparation method thereof |
| CN110743393A (en) * | 2019-11-19 | 2020-02-04 | 北京林业大学 | Preparation of lignin-based polyarylester composite nanofiltration membrane |
| CN111450717B (en) * | 2020-04-24 | 2022-03-22 | 北京工业大学 | High-performance polymer organic solvent nanofiltration membrane and preparation method thereof |
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