CN109569308B - Preparation method for preparing high-flux reverse osmosis membrane by acid absorbent system - Google Patents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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- B01D67/0088—Physical treatment with compounds, e.g. swelling, coating or impregnation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/441—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by reverse osmosis
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/08—Seawater, e.g. for desalination
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Abstract
A method for preparing a high-flux reverse osmosis membrane by using an acid acceptor system. The invention discloses the technical field of reverse osmosis composite membranes, and discloses a preparation method of a high-flux seawater membrane based on a novel buffer system. The invention firstly coats a water phase solution containing polyamine and one or more weak acid salts or weak acid and tetramethyl ammonium hydroxide on a polysulfone basement membrane, then coats an oil phase solution in which polyacyl chloride is dissolved in Isopar G (1 isoalkane solvent) after drying in the shade, and then carries out post-treatment on the coated membrane at a certain temperature to finally obtain the reverse osmosis seawater membrane. Wherein the aqueous phase of the coating solution comprises one or more ammonium salts dissolved in water. Compared with the prior art, the invention has the advantages of simple and easily controlled buffering, good retention rate, greatly improved water flux, good reproducibility and low preparation cost.
Description
Technical Field
The invention belongs to the technical field of reverse osmosis composite membranes, and relates to a preparation method of a high-flux seawater membrane based on a novel buffer system.
Background
Water flux is one of the most important properties of reverse osmosis membranes. Higher water flux means lower energy consumption for treating the same volume of liquid. The reverse osmosis mainly goes through two stages, Loeb and Sourirajan develop the manufacturing method of the asymmetric membrane in 1960, the removal rate of the prepared membrane to the salt is 98.6 percent under 10MPa, and the water permeability reaches 10.8 LMH. Subsequently, the pressure difference across the membrane is reduced, and the water flux is always the most main target of the desalination membrane for pursuing high performance. The first composite membrane was prepared by j.e.cadotte polymerization at the end of the 70 s, and became a milestone for the development of low-pressure high-flux desalination membranes.
The current ultra-low pressure reverse osmosis or nanofiltration membrane has the operating pressure of less than 0.5MPa and the water flux of 30-60 LMH. The research of the ultra-low pressure high flux reverse osmosis composite membrane is an important target of the researchers to research the composite membrane. The reverse osmosis membrane is generally prepared by interfacial polymerization of polyamine and acyl chloride, in the interfacial reaction, the polyamine and the acyl chloride are subjected to polycondensation reaction to generate polyamide and simultaneously generate hydrogen chloride as a side reaction, accumulation of the hydrogen chloride in a reaction zone can limit forward progress of the polycondensation reaction, so that an appropriate buffer system is selected to remove the hydrogen chloride in the reaction, and an active separation layer with higher molecular weight is formed, so that the separation membrane with higher retention rate is prepared. Koo et al have studied different systems of acid scavengers, and the composite membrane prepared using a camphorsulfonic acid (CSA)/Triethylamine (TEA) system of acid scavengers has the most excellent performance. Still other researchers have used triethylamine hydrochloride and camphorsulfonic acid (CSA)/Triethylamine (TEA) systems together as acid scavengers and have also produced composite membranes with superior performance. In general, basic chemical substances can be used as acid-absorbing agents, and the promoting mechanism of the basic chemical substances on interfacial polymerization is as follows: taking triethylamine as an example, triethylamine molecules and m-phenylenediamine molecules diffuse together from the aqueous phase into a reaction zone located in the organic phase, and due to the low reactivity of triethylamine and acyl chloride, triethylamine reacts only with hydrogen chloride to produce ammonium salt, but not with acyl chloride, and the produced ammonium salt is insoluble in the organic phase, thereby bringing the byproduct hydrogen chloride out of the reaction zone. However, the addition of an acid-acceptor increases the pH of the reaction system, and an excessively high pH accelerates the hydrolysis of the acid chloride, so that one or more acidic substances (pH adjusting agents) should be added to adjust the pH of the system at the same time as the addition of the acid-acceptor. Generally, the buffer system is basically a mixed solution composed of a weak acid and its salt, a weak base and its salt. The tetramethylammonium hydroxide has strong basicity and a boiling point of 120 ℃, is easily decomposed into trimethylamine and methanol when heated to the boiling point, and the heat treatment temperature generally exceeds 120 ℃ in the preparation process of the seawater membrane. Therefore, tetramethylammonium hydroxide is added into a buffer system, the alkalinity is slowly weakened in the heat treatment process, and trimethylamine generated by decomposition can form a new buffer system with weak acid salts or weak acids in the system. In the invention, a buffer system containing tetramethylammonium hydroxide and weak acid is adopted to prepare the high-flux seawater film. When the heat treatment temperature is above 120 ℃, the pH value of the system is higher and the alkalinity is higher at the moment of entering the heat treatment, so the reaction is faster, the formed compact layer is also more compact, the pH value of the system is reduced along with the passage of time, the reaction trend is gentle, trimethylamine and methanol can be generated during the decomposition of tetramethylammonium hydroxide and can escape from the separation layer, the structure of the separation layer can be adjusted to a certain degree, and the water flux is improved. The research of the invention is to use a buffer system containing tetramethyl ammonium hydroxide and weak acid salts or weak acids to prepare the seawater film and improve the water flux of the seawater film.
Disclosure of Invention
The invention aims to provide a novel buffer system for preparing a high-flux seawater film and a preparation method thereof. In the research, one or more weak acid salts or weak acid and tetramethyl ammonium hydroxide are added in the interfacial polymerization reaction to serve as a buffer system for the reaction. The preparation process of the novel high-flux seawater membrane comprises the steps of firstly coating a water phase solution containing polyamine and one or more weak acid salts or weak acids and tetramethyl ammonium hydroxide on a polysulfone bottom membrane, then coating an oil phase solution in which polyacyl chloride is dissolved in Isopar L (1 isoparaffin solvent), and preparing the high-flux seawater membrane through interfacial polymerization. By optimally selecting various components and types of the coating liquid and regulating and controlling the post-treatment temperature, the seawater film with high water flux is prepared.
The invention is realized by the following technical scheme:
a preparation method for preparing a high-flux reverse osmosis membrane by using a novel acid acceptor system is characterized by comprising the following steps: firstly coating a water phase solution containing polyamine and one or more weak acid salts or weak acid and tetramethyl ammonium hydroxide on a polysulfone basement membrane, drying in the shade, then coating an oil phase solution in which polyacyl chloride is dissolved in Isopar G (1 isoalkane solvent), and then carrying out post-treatment on the coated membrane at a certain temperature to finally obtain the reverse osmosis seawater membrane. Wherein the aqueous phase of the coating solution comprises one or more ammonium salts dissolved in water.
Preferably, in the above preparation method, the polymer contained in the aqueous phase solution is one or more of metaphenylene diamine (MPD), piperazine (PIP) and polyethyleneimine, and the mass percentage of the polymer in the aqueous phase is 0.1-5.0%. The aqueous phase solution can contain one or more of tetramethylammonium hydroxide, ammonium chloride, tetraethylammonium chloride, boric acid, citric acid and triethylamine hydrochloride, and the mass percent of the ammonium salt in the aqueous phase is 0.1-10%. More preferably, the polymer of the aqueous phase solution is m-phenylenediamine (MPD), and the mass percent of the m-phenylenediamine (MPD) is 0.1-3%. Preferably, the mass percent of the tetramethylammonium hydroxide in the water phase is 0.1-5%.
Preferably, in the above preparation method, the polymer contained in the oil phase solution is one or more of trimesoyl chloride (TMC), adipoyl chloride (APC), and Hexamethylene Diisocyanate (HDI), and the mass percentage of the polymer solute in the oil phase is 0.1-4.0%. More preferably, the polymer in the oil phase solution is trimesoyl chloride (TMC), and the TMC accounts for 0.1-3.5% by mass.
Preferably, the weak acid salt or weak acid in the preparation method is one or more of ammonium chloride, boric acid and triethylamine hydrochloride, and the mass percentage of the water phase is 0.1-6%.
Preferably, the post-treatment temperature of the composite membrane in the preparation method is 100-150 ℃. More preferably, the post-treatment temperature of the reverse osmosis membrane is 120-140 ℃.
In the invention, the polysulfone base film can be any base film provided by manufacturers, and the performance difference of the base film and the type of the base film have no direct influence on the result of the invention, so that the commercial polysulfone base film can be selected or made by self, which also provides possibility for common application and commercial application of the invention.
In the invention, the raw materials of the novel buffer system are easy to obtain, and all components are very soluble in water, so that any production process of a production line is not changed in the production process of the production line, thereby providing possibility for common application and commercial application of the invention.
The post-treatment temperature of the reverse osmosis seawater film can be controlled by an oven, and the performance is superior particularly at 120-140 ℃.
Has the beneficial effects that: by adopting the method disclosed by the patent, the high-flux reverse osmosis seawater film with excellent interception performance can be prepared by only adding tetramethylammonium hydroxide and one or more weakly acidic substances through an interfacial polymerization method. Compared with the prior art, the novel water-saving filter has the advantages that the buffer is simple and easy to control, the good interception rate is kept, the water flux is greatly improved, the reproducibility is good, and the preparation cost is low.
Detailed Description
The following is a detailed description of embodiments of the invention:
the following example presents a method for the preparation of a high flux seawater membrane based on a novel buffer system. The following examples are provided by way of illustration only and are not intended to limit the invention.
The polysulfone base film used in the following examples is a self-made base film. The film production date was less than 30 days to the experimental date, during which time it was stored in 2% aqueous sodium bisulfite. Before the interfacial reaction is carried out to prepare the composite membrane, the polysulfone base membrane is soaked in pure water 24 hours in advance.
The evaluation of the membrane performance of high flux reverse osmosis membranes based on the novel acid scavenger system is made in the following examples: sodium chloride salt rejection and water flux. The test pressure during performance evaluation is 550psi, the flow rate of the concentrated water is 1.0L/min, the ambient temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, and the concentrated water is an aqueous solution of sodium chloride and has the concentration of 32000 ppm.
In the following examples, the salt rejection is defined as the difference between the concentrations of concentrate and product water divided by the concentrate concentration; the water flux is defined as the volume of water per unit time that permeates the composite separation membrane per unit area in the above test procedure and is expressed in L/m2H (LMH). Each data point above was averaged from 9 samples.
Comparative example
Different reverse osmosis seawater membranes were prepared by continuously changing the aqueous and oil phase solubility and the oven post-treatment temperature, but using the most common buffer system triethylamine hydrochloride/triethylamine system. Through experimental tests, the rejection rate of the prepared reverse osmosis membrane to 32000ppm sodium chloride aqueous solution is up to 99.6%, and the water flux is up to 55 LMH. The test pressure during performance evaluation is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, and the concentrated water is a sodium chloride aqueous solution with the concentration of 32000 ppm.
Example 1
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding 1% of tetramethylammonium hydroxide and 1% of ammonium chloride, uniformly mixing, and preparing 0.2% of trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 120 ℃ oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 65LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 2
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding 1.5% of tetramethylammonium hydroxide and 1% of ammonium chloride, uniformly mixing, and preparing 0.2% of trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60 seconds, drying in the shade, coating the oil phase solution on the membrane dried in the shade, pouring off the redundant oil phase solution after 30 seconds, and carrying out heat treatment for 5min in a 130 ℃ drying oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 68LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 3
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 1% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing trimesoyl chloride (TMC) oil phase solution with the mass fraction of 0.3%. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 120 ℃ oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 62LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 4
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding 1% of tetramethylammonium hydroxide and 2% of ammonium chloride, uniformly mixing, and preparing 0.2% of trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 120 ℃ oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 70LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 5
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 2% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing 0.3% trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 120 ℃ oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 72LMH and the desalination rate of 99.7 percent under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 6
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 2.5% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing trimesoyl chloride (TMC) oil phase solution with the mass fraction of 0.2%. Firstly coating a water phase solution on a polysulfone bottom membrane, pouring off the redundant solution after 60s, drying in the shade, coating an oil phase solution on the membrane dried in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 120 ℃ drying oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 75LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 7
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 3% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing 0.2% trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a drying oven at 140 ℃. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 78LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 8
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 4% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing trimesoyl chloride (TMC) oil phase solution with the mass fraction of 0.2%. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 5min in a 130 ℃ oven. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 75LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Example 9
Preparing m-phenylenediamine aqueous solution with the mass fraction of 3%, adding tetramethyl ammonium hydroxide with the mass fraction of 4% and ammonium chloride with the mass fraction of 1%, uniformly mixing, and preparing 0.3% trimesoyl chloride (TMC) oil phase solution. Firstly coating the polysulfone basement membrane with the aqueous phase solution, pouring off the redundant solution after 60s, drying in the shade, coating the oil phase solution on the dried membrane in the shade, pouring off the redundant oil phase solution after 30s, and carrying out heat treatment for 3min in a drying oven at 140 ℃. The high-flux seawater membrane based on the novel buffer system prepared by the method has the water flux of 78LMH and the desalination rate of 99.7% under the experimental conditions that the test pressure is 550psi, the concentrated water flow is 1.0L/min, the environmental temperature is 25 ℃, the pH value of the concentrated water is 6.5-7.5, the concentrated water is a sodium chloride aqueous solution and the concentration is 32000 ppm.
Claims (1)
1. A method for preparing a high-flux reverse osmosis membrane by an acid absorbent system is characterized by comprising the following steps: firstly coating a layer of aqueous phase solution on a polysulfone basement membrane, wherein the aqueous phase solution contains tetramethyl ammonium hydroxide, ammonium chloride and m-phenylenediamine; after drying in the shade, coating an oil phase solution, wherein the oil phase solution is a solution of trimesoyl chloride dissolved in Isopar G;
then, carrying out post-treatment on the coated membrane to finally obtain a reverse osmosis seawater membrane;
wherein the mass percent of the tetramethylammonium hydroxide in the aqueous phase solution is 3%, the mass percent of the ammonium chloride in the aqueous phase solution is 1%, the mass percent of the m-phenylenediamine in the aqueous phase solution is 3%, the mass percent of the trimesoyl chloride in the oil phase solution is 0.2%, the post-treatment temperature is 140 ℃, and the time is 5min,
or the mass percent of the tetramethylammonium hydroxide in the aqueous phase solution is 4%, the mass percent of the ammonium chloride in the aqueous phase solution is 1%, the mass percent of the m-phenylenediamine in the aqueous phase solution is 3%, the mass percent of the trimesoyl chloride in the oil phase solution is 0.3%, the temperature for post-treatment is 140 ℃, and the time is 3 min.
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| CN111450714A (en) * | 2020-04-17 | 2020-07-28 | 蓝星（杭州）膜工业有限公司 | Method for preparing composite nanofiltration membrane by using multi-element buffer system |
| CN112827369B (en) * | 2021-01-18 | 2021-11-09 | 蓝星（杭州）膜工业有限公司 | Preparation method of nano hybrid composite membrane |
| CN112808021B (en) * | 2021-01-18 | 2021-11-09 | 杭州水处理技术研究开发中心有限公司 | Method for preparing reverse osmosis membrane by adopting novel water phase system |
| CN115155323A (en) * | 2022-07-22 | 2022-10-11 | 青岛沁安化工科技有限公司 | Reverse osmosis and forward osmosis membrane repairing agent and preparation method thereof |
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