CN112717721B - Acid-resistant composite nanofiltration membrane and preparation method thereof - Google Patents
Acid-resistant composite nanofiltration membrane and preparation method thereof Download PDFInfo
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- CN112717721B CN112717721B CN202011559527.XA CN202011559527A CN112717721B CN 112717721 B CN112717721 B CN 112717721B CN 202011559527 A CN202011559527 A CN 202011559527A CN 112717721 B CN112717721 B CN 112717721B
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/02—Reverse osmosis; Hyperfiltration ; Nanofiltration
- B01D61/027—Nanofiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/14—Ultrafiltration; Microfiltration
- B01D61/145—Ultrafiltration
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/10—Supported membranes; Membrane supports
- B01D69/105—Support pretreatment
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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
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2323/00—Details relating to membrane preparation
- B01D2323/12—Specific ratios of components used
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/124—Water desalination
- Y02A20/131—Reverse-osmosis
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Abstract
The invention provides an acid-resistant composite nanofiltration membrane which is characterized by comprising a support base layer and a functional layer obtained on the support base layer through interfacial polymerization, wherein the functional layer comprises the following raw material components: the oil-phase solvent comprises amine substances, a water-phase additive, cyanuric chloride, polyacyl chloride, an oil-phase solvent and deionized water, wherein the amine substances comprise piperazine and ethylene amine substances. The acid-resistant composite nanofiltration membrane prepared by the invention has the water flux reaching 26.39LMH before the soaking treatment of the hydrochloric acid solution with the mass fraction of 10%, the rejection rate of divalent salt reaching 97.71%, and the water flux reaching 28.22LMH and the rejection rate of divalent salt reaching 96.28% after the soaking treatment of the hydrochloric acid solution with the mass fraction of 10%. The preparation method is simple and easy to implement, short in process flow, low in cost and good in application prospect.
Description
Technical Field
The invention relates to the technical field of nanofiltration membrane preparation, and particularly relates to an acid-resistant composite nanofiltration membrane and a preparation method thereof.
Background
The excellent separation performance of the composite nanofiltration membrane is always paid extensive attention by academia and industry. The composite nanofiltration membrane can not only separate gradient interception of different inorganic salts, but also accurately separate substances with molecular weight of 200-1000.
The composite nanofiltration membrane is often used for separating and purifying foods and biological products, and is very easy to be polluted by biomolecules and microorganisms, so that the composite nanofiltration membrane is often cleaned by acid cleaning solution, and the composite nanofiltration membrane is required to have certain acid resistance, so that the use frequency of the composite nanofiltration membrane is increased. In the fields of metal and electroplating, acid is commonly used for cleaning, etching, demolding and other processes of metal surfaces, so that a large amount of acid solution and metal ions dissolved in the acid solution are generated. The acid-resistant composite nanofiltration membrane has good acid permeability and metal ion interception, and can effectively realize the recovery of acid and metal ions. In the paper making and printing industry, acid waste liquid can be discharged, and the acid-resistant composite nanofiltration membrane can effectively treat acid sewage and recover inorganic acid. The acid-resistant composite nanofiltration membrane can effectively reduce the chemical oxygen demand of acidic sewage when the acidic sewage generated by soil cleaning is treated.
At present, the composite nanofiltration membrane used in the market has the problems of low water flux and poor acid resistance. Therefore, an acid-resistant composite nanofiltration membrane and a preparation method thereof are urgently needed to solve the problems in the prior art.
Disclosure of Invention
The invention aims to provide an acid-resistant composite nanofiltration membrane and a preparation method thereof, and the specific technical scheme is as follows:
an acid-resistant composite nanofiltration membrane comprises a supporting base layer and a functional layer obtained by interfacial polymerization on the supporting base layer, wherein the functional layer comprises the following raw material components: the oil-phase solvent comprises amine substances, a water-phase additive, cyanuric chloride, polyacyl chloride, an oil-phase solvent and deionized water, wherein the amine substances comprise piperazine and ethylene amine substances.
Preferably, the ethylene amine includes at least one of ethylene diamine, diethylene triamine, triethylene tetramine, tetraethylene pentamine and pentaethylene hexamine.
Preferably, the poly-acid chloride comprises at least one of trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride, terephthaloyl chloride, 4,4' -biphenylacetyl chloride, succinyl chloride, glutaryl dichloride, adipoyl chloride, and 1,4-cyclohexanedicarboxylic acid chloride.
Preferably, the water phase additive comprises at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, ammonium lauryl sulfate and sodium hydroxyethyl sulfonate;
the oil phase solvent is n-hexane.
Preferably, the support base layer comprises a non-woven fabric and a porous ultrafiltration layer, the non-woven fabric is made of at least one of polyester, polypropylene and polyethylene, and the porous ultrafiltration layer is made of at least one of polysulfone, polyethersulfone, sulfonated polyethersulfone and polyacrylonitrile.
The preparation method of the acid-resistant composite nanofiltration membrane comprises the following steps,
preparing aqueous phase solution
The amine substance, the water phase additive and the deionized water are mixed according to the mass ratio of (0.1-5): (0.01-0.1): (94.9-99.89), and uniformly mixing to prepare an aqueous phase solution;
preparing oil phase solution
The cyanuric chloride, the polyacyl chloride and the oil phase solvent are mixed according to the mass ratio of (0.01-3): (0.01-3): (94-99.98), and uniformly mixing to prepare an oil phase solution;
preparation of acid-resistant composite nanofiltration membrane
And immersing the support base layer into the water-phase solution for 15-25s, immersing the immersed support base layer into the oil-phase solution for 10-20s, and performing heat treatment to obtain the acid-resistant composite nanofiltration membrane.
Preferably, the heat treatment is performed in an oven at 30-90 deg.C for 1-30min.
Preferably, in the aqueous solution, the mass ratio of the piperazine to the ethylene amine is 1: (0.1-10).
Preferably, the residual aqueous solution on the surface of the support base layer after the support base layer is soaked in the aqueous solution is removed by a rubber roller.
Preferably, the oil phase solution remained on the surface of the support base layer after the support base layer is soaked by the oil phase solution is removed by a rubber roller.
The technical scheme of the invention has the following beneficial effects:
(1) The acid-resistant composite nanofiltration membrane disclosed by the invention not only forms a polyamide structure through interfacial polycondensation of piperazine and polyacyl chloride, but also is added with an ethylene amine substance, wherein the ethylene amine substance contains primary amine (-NH 2) and secondary amine (-NH-), and the primary amine has high reaction activity, so that the ethylene amine substance can be ensured to react with cyanuric chloride and polyacyl chloride at room temperature. Secondary amines, while less reactive than primary amines, are also capable of reacting with cyanuric chloride and polyacyl chloride at suitable temperatures. Therefore, when the acid-resistant composite nanofiltration membrane is industrially produced, the reaction can be continuously and effectively carried out even if the equipment temperature cannot reach the reaction temperature in time. Compared with piperazine, the ethylene amine substance can also increase the crosslinking degree after the reaction with cyanuric chloride and polyacyl chloride, and form the three-position netted acid-resistant composite nanofiltration membrane with stable structure. Under the environment of an acid solution, the acid-resistant composite nanofiltration membrane has better acid degradation resistance. In addition, the ethylene amine substance is cheap and easy to obtain, and the production cost is saved. The invention uses cyanuric chloride to participate in interfacial polymerization, introduces C-N bond into the molecule of the acid-resistant composite nanofiltration membrane, and because the radius of N atom is less than that of C atom, the energy of C-N bond is more than that of C-C bond. The introduction of the C-N bond greatly improves the stability of the molecules of the acid-resistant composite nanofiltration membrane, and further improves the acid resistance of the acid-resistant composite nanofiltration membrane. The acid-resistant composite nanofiltration membrane prepared by the invention has the water flux reaching 26.39LMH before the soaking treatment of the hydrochloric acid solution with the mass fraction of 10%, the rejection rate of divalent salt reaching 97.71%, and the water flux reaching 28.22LMH and the rejection rate of divalent salt reaching 96.28% after the soaking treatment of the hydrochloric acid solution with the mass fraction of 10%.
(2) The preparation method of the acid-resistant composite nanofiltration membrane is simple and easy to implement, short in process flow, low in cost and good in application prospect.
Detailed Description
The following is a detailed description of embodiments of the invention, but the invention can be implemented in many different ways, as defined and covered by the claims.
Example 1:
an acid-resistant composite nanofiltration membrane, comprising a support base layer and a functional layer obtained by interfacial polymerization on the support base layer, wherein the functional layer comprises the following raw material components: the oil-phase solvent comprises amine substances, a water-phase additive, cyanuric chloride, polyacyl chloride, an oil-phase solvent and deionized water, wherein the amine substances comprise piperazine and ethylene amine substances.
The ethylene amine substance is triethylene tetramine.
The polybasic acyl chloride is trimesoyl chloride.
The water phase additive is sodium dodecyl sulfate;
the oil phase solvent is n-hexane.
The support basic unit includes non-woven fabrics and porous ultrafiltration layer, the material of non-woven fabrics is polypropylene, the material of porous ultrafiltration layer is polyethersulfone.
The preparation process of the supporting base layer comprises the following steps: 75g of polyether sulfone resin (PES) and 425g of N-methylpyrrolidone (NMP) are weighed, mixed and prepared into 500g of solution, and stirred for 6 hours at 70 ℃ to prepare evenly dispersed membrane casting solution. Filtering the membrane casting solution, vacuum degassing, uniformly coating on a non-woven fabric on a membrane scraping machine, wherein the wet membrane thickness is 150 mu m, evaporating at room temperature for 3s, immersing in ultrapure water at 16 ℃ for gel curing to form a membrane, completely curing the membrane by normal temperature water, finally treating the membrane in water at 75 ℃ for 3min to obtain a support base layer, and refrigerating in a freezer at 5 ℃ for later use.
The preparation method of the acid-resistant composite nanofiltration membrane comprises the following steps,
preparing aqueous phase solution
And (2) mixing the amine substance, the water-phase additive and deionized water according to the mass ratio of 1:0.02:98.98, and evenly mixing to prepare an aqueous phase solution;
preparing oil phase solution
The cyanuric chloride, the polyacyl chloride and the oil phase solvent are mixed according to the mass ratio of 0.2:0.01:99.79, and evenly mixing to prepare an oil phase solution;
preparation of acid-resistant composite nanofiltration membrane
And immersing the support base layer into the water phase solution for 20s, immersing the immersed support base layer into the oil phase solution for 15s, and performing heat treatment to obtain the acid-resistant composite nanofiltration membrane.
The heat treatment is carried out in an oven at 70 ℃ for 5min.
In the preparation of the aqueous solution, the mass ratio of the piperazine to the ethylene amine substances is 1:10.
and removing the residual aqueous phase solution on the surface of the support base layer by using a rubber roller after the support base layer is soaked by the aqueous phase solution.
And removing the residual oil phase solution on the surface of the support base layer by using a rubber roller after the support base layer is soaked by the oil phase solution.
Example 2:
the difference from example 1 is that the ethyleneamine is diethylenetriamine.
Example 3:
the difference from example 1 is that the ethyleneamine is tetraethylenepentamine.
Example 4:
the difference from example 1 is that the mass ratio of piperazine to triethylenetetramine is 1:2.
Example 5:
the difference from example 1 is that the mass ratio of piperazine to triethylenetetramine is 1:1.
Example 6:
the difference from example 1 is that the mass ratio of piperazine to triethylenetetramine is 2:1.
Example 7:
the difference from the example 4 is that the mass ratio of the cyanuric chloride to the trimesoyl chloride is 2:1.
Example 8:
the difference from example 4 is that the mass ratio of cyanuric chloride to trimesoyl chloride is 1:1.
Example 9:
the difference from the example 4 is that the mass ratio of the cyanuric chloride to the trimesoyl chloride is 1:2.
Comparative example 1:
except that the amount of the cyanuric chloride added was zero as in example 1.
Comparative example 2:
the difference from example 1 is that the amount of the ethyleneamines added is zero.
Comparative example 3:
the difference from example 4 is that the addition amount of cyanuric chloride is zero.
The acid-resistant composite nanofiltration membranes prepared in examples 1 to 9 and comparative examples 1 to 3 were tested for acid resistance by the following test methods: and (3) carrying out two tests on the acid-resistant composite nanofiltration membrane on a cross-flow type membrane detection table, wherein the tests are respectively the performance test before the hydrochloric acid solution soaking treatment and after the hydrochloric acid solution soaking treatment. The test conditions were: mgSO (MgSO) 4 The aqueous solution had a concentration of 2000ppm, an operating pressure of 70psi, a test temperature of 25 deg.C and a pH of 6.5-7.5. The hydrochloric acid solution soaking treatment specifically adopts a hydrochloric acid solution with the mass concentration of 10%, the soaking time is one week, and the temperature of the hydrochloric acid solution is 25 ℃. See table 1 for specific test results.
TABLE 1 Performance test of acid-resistant composite nanofiltration membranes prepared in examples 1 to 9 and comparative examples 1 to 3
As shown in the data in Table 1, compared with the data in comparative examples 1 to 3, the acid-resistant composite nanofiltration membranes prepared in examples 1 to 9 have good water flux and rejection rate before and after the soaking treatment in the hydrochloric acid solution, which indicates that the acid-resistant composite nanofiltration membranes prepared in the invention have good acid resistance. From examples 4 to 6, it is known that the water flux of the acid-resistant composite nanofiltration membrane can be increased with the increase of the piperazine proportion, but the acid resistance is decreased because the rejection rate is decreased after the hydrochloric acid solution immersion treatment. From examples 7 to 9, it is known that the increase of the percentage of trimesoyl chloride can increase the water flux of the acid-resistant composite nanofiltration membrane, but the retention rate is reduced after the soaking treatment with the hydrochloric acid solution, so the acid resistance is reduced. From example 8, it is known that the water flux and acid resistance of the acid-resistant composite nanofiltration membrane prepared when the mass ratio of the cyanuric chloride to the trimesoyl chloride is 1:1 are optimal. From the comparative examples 2 to 3, it is known that when only piperazine is in the water phase or only trimesoyl chloride is in the oil phase, the retention rate of the acid-resistant composite nanofiltration membrane after the hydrochloric acid solution soaking treatment is basically maintained at about 86%, which is obviously lower than the retention rate of the acid-resistant composite nanofiltration membrane before the hydrochloric acid solution soaking treatment, so that the acid resistance of the acid-resistant composite nanofiltration membrane prepared by the comparative examples 2 to 3 is not obviously improved.
In conclusion, the acid-resistant composite nanofiltration membrane prepared by the method disclosed by the invention is beneficial to efficiently intercepting inorganic salt, the treatment efficiency of waste acid is improved, and the market application of the acid-resistant composite nanofiltration membrane in the aspect of waste acid recovery is increased.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. An acid-resistant composite nanofiltration membrane, which is characterized by comprising a support base layer and a functional layer obtained by interfacial polymerization on the support base layer, wherein the functional layer comprises the following raw material components: the oil-phase solvent comprises amine substances, a water-phase additive, cyanuric chloride, polyacyl chloride, an oil-phase solvent and deionized water, wherein the amine substances comprise piperazine and ethylene amine substances; the mass ratio of the piperazine to the ethylene amine is 1: (0.1-10);
the ethylene amine substance comprises at least one of ethylene diamine, diethylenetriamine, triethylene tetramine, tetraethylenepentamine and pentaethylene hexamine;
the water phase additive comprises at least one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate, ammonium lauryl sulfate and sodium hydroxyethyl sulfonate.
2. The acid resistant composite nanofiltration membrane of claim 1, wherein the polyacyl chloride comprises at least one of trimesoyl chloride, phthaloyl chloride, isophthaloyl chloride, terephthaloyl chloride, 4,4' -biphenylacetyl chloride, succinoyl chloride, glutaryl dichloride, adipoyl chloride, and 1,4-cyclohexanedicarboxylic acid chloride.
3. The acid-resistant composite nanofiltration membrane according to claim 1, wherein the oil-phase solvent is n-hexane.
4. The acid-resistant composite nanofiltration membrane according to claim 1, wherein the support base layer comprises a non-woven fabric and a porous ultrafiltration layer, the non-woven fabric comprises at least one of polyester, polypropylene and polyethylene, and the porous ultrafiltration layer comprises at least one of polysulfone, polyethersulfone, sulfonated polyethersulfone and polyacrylonitrile.
5. The preparation method of the acid-resistant composite nanofiltration membrane according to any one of claims 1 to 4, comprising the following steps,
preparing aqueous phase solution
The amine substance, the water phase additive and the deionized water are mixed according to the mass ratio of (0.1-5): (0.01-0.1): (94.9-99.89), and uniformly mixing to prepare an aqueous phase solution;
preparing oil phase solution
The cyanuric chloride, the polyacyl chloride and the oil phase solvent are mixed according to the mass ratio of (0.01-3): (0.01-3): (94-99.98), and uniformly mixing to prepare an oil phase solution;
preparation of acid-resistant composite nanofiltration membrane
And immersing the support base layer into the water-phase solution for 15-25s, immersing the immersed support base layer into the oil-phase solution for 10-20s, and performing heat treatment to obtain the acid-resistant composite nanofiltration membrane.
6. The method of claim 5, wherein the heat treatment is performed in an oven at 30-90 ℃ for 1-30min.
7. The method according to claim 6, wherein the residual aqueous solution on the surface of the support substrate is removed by a rubber roller after the support substrate is soaked in the aqueous solution.
8. The method according to claim 7, wherein the oil phase solution remaining on the surface of the support base layer after the support base layer is soaked in the oil phase solution is removed by using a rubber roller.
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| CN113856488A (en) * | 2021-11-08 | 2021-12-31 | 湖南澳维环保科技有限公司 | Composite nanofiltration membrane and preparation method thereof |
| CN114307695A (en) * | 2021-12-17 | 2022-04-12 | 沃顿科技股份有限公司 | Chlorine-resistant composite reverse osmosis membrane and preparation method thereof |
| CN114950135B (en) * | 2022-06-24 | 2024-01-26 | 中国科学院青海盐湖研究所 | Acid-resistant nanofiltration membrane, and preparation method and application thereof |
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| WO1991011250A1 (en) * | 1990-01-26 | 1991-08-08 | Toray Industries, Inc. | Composite semipermeable membrane and production thereof |
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| CN105617875A (en) * | 2014-11-03 | 2016-06-01 | 株洲时代新材料科技股份有限公司 | High-throughput hollow fiber composite nanofiltration membrane, and preparation method thereof |
| CN107349804A (en) * | 2017-07-13 | 2017-11-17 | 中国科学院生态环境研究中心 | A kind of preparation method of high flux anti-acid NF membrane |
| CN107899436A (en) * | 2017-11-24 | 2018-04-13 | 贵阳时代沃顿科技有限公司 | A kind of preparation method of the alkaline-resisting NF membrane of high-performance |
| KR102157932B1 (en) * | 2017-12-22 | 2020-09-18 | 주식회사 엘지화학 | Method for manufacturing water-treatment separation membrane, water-treatment separation membrane manufactured by thereof, and composition for manufacturing water-treatment separation membrane |
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