CN113318610A - Desalting membrane for removing COD (chemical oxygen demand) and preparation method thereof - Google Patents
Desalting membrane for removing COD (chemical oxygen demand) and preparation method thereof Download PDFInfo
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- CN113318610A CN113318610A CN202110505770.1A CN202110505770A CN113318610A CN 113318610 A CN113318610 A CN 113318610A CN 202110505770 A CN202110505770 A CN 202110505770A CN 113318610 A CN113318610 A CN 113318610A
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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
- B01D69/08—Hollow fibre membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D67/00—Processes specially adapted for manufacturing semi-permeable membranes for separation processes or apparatus
- B01D67/0002—Organic membrane manufacture
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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
- B01D69/02—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor characterised by their properties
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2325/00—Details relating to properties of membranes
- B01D2325/30—Chemical resistance
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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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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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Organic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention provides a desalting membrane for removing COD (chemical oxygen demand) and a preparation method thereof, wherein the desalting membrane is mainly prepared from a base membrane, a modifier and a curing agent, and the base membrane is mainly prepared from the following raw materials: the composite material comprises, by mass, 25-35 parts of polymer resin powder, 55-65 parts of N, N-dimethylacetamide, 1-5 parts of an additive and 5-10 parts of a pore-forming agent. The desalting membrane prepared by the invention has good water flux, and simultaneously has higher desalting rate and COD removal rate.
Description
Technical Field
The invention relates to the field of desalting membranes, in particular to a desalting membrane for removing COD (chemical oxygen demand) and a preparation method thereof.
Background
Along with the increase of population, the water demand approaches the water resource and can be developed and utilized, and the problem of water shortage is more prominent. Meanwhile, with the rapid development of economy, the problems of water resource pollution and shortage caused by the rapid development of economy are increasingly highlighted. Among the wastewaters, industrial wastewater refers to wastewater and sewage produced in industrial production activities. Nowadays, the nation pays more and more attention to the treatment of industrial wastewater, the treatment means of industrial wastewater are more and more, and the market scale is continuously enlarged. Among them, the advantage of using the membrane technology is to recover useful substances in industrial wastewater and to be able to reuse the recovered water, which makes membrane separation technology widely paid attention. The method can help greatly reduce the discharge amount of industrial wastewater, and even realize zero discharge of the wastewater. In recent years, the membrane separation technology has received attention of a large number of researchers by virtue of the characteristics of high separation efficiency, low energy consumption, low material consumption, simple process, convenient operation and no secondary pollution.
The method is classified according to production objects in different industrial industries and mainly comprises papermaking wastewater, chemical fertilizer wastewater, leather-making wastewater, metallurgical wastewater, textile wastewater, power station wastewater, coking gas wastewater, petrochemical wastewater and the like. The waste water from textile industry features high COD value, and contains inorganic salts and suspended matter. The textile industry wastewater can adopt a membrane treatment technology to realize the purposes of removing colored dyes in the wastewater and recycling the production water. However, the existing membrane has low treatment efficiency and general treatment effect.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a desalting membrane with a simple formula, which has good water flux and high desalting rate and COD removal rate.
The second purpose of the invention is to provide the preparation method of the desalting membrane, which has the advantages of simple operation, mild operation conditions, no pollution, no discharge of three wastes, safety and environmental protection.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the invention provides a desalting membrane which is mainly prepared from a base membrane, a modifier and a curing agent, wherein the base membrane is mainly prepared from the following raw materials: the composite material comprises, by mass, 25-35 parts of polymer resin powder, 55-65 parts of N, N-dimethylacetamide, 1-5 parts of an additive and 5-10 parts of a pore-forming agent.
In the prior art, more and more printing and dyeing enterprises advocate energy conservation and emission reduction, and hopefully, COD can be retained in the process of recycling printing and dyeing wastewater, and salt ions permeate the COD so as to realize recycling. Based on this requirement, development of relevant properties of hollow fiber membranes is required.
In order to solve the technical problems, the invention provides a desalination membrane, and firstly, a hollow fiber membrane has an effect of intercepting organic pollutants. Secondly, the hollow fiber membrane can enrich organic degradation bacteria and degrade organic matters which are difficult to degrade. Finally, the hollow fiber membrane has good acid-base resistance and pollution resistance. When the hollow fiber membrane is used for treating wastewater, the hollow fiber membrane has the advantages of stable effluent quality, high treatment efficiency and the like.
Preferably, as a further implementable scheme, by mass, 30-32 parts of polymer resin powder, 57-62 parts of N, N-dimethylacetamide, 2-4 parts of an additive and 6-8 parts of a pore-forming agent.
Preferably, as a further implementable scheme, the polymer resin comprises, by mass, 31 parts of polymer resin powder, 60 parts of N, N-dimethylacetamide, 3 parts of an additive and 7 parts of a pore-forming agent.
In the formula of the desalting membrane, polymer resin powder and N, N-dimethylacetamide are subjected to a good synergistic compatibility effect, wherein the polymer resin powder has a strong absorption effect, can absorb hundreds of times and even thousands of times of water of the polymer resin powder by weight and has a strong water retention capacity, so that the desalting membrane has a quite remarkable effect of improving the water flux of the membrane, and the polymer resin powder is preferably one of polysulfone, polyethersulfone or polyvinylidene fluoride.
N, N-dimethylacetamide is used as a solvent, so that the N, N-dimethylacetamide has strong dissolving property with high molecular substances, and is more favorable for the dispersion uniformity of high molecular resin powder, thereby improving the stability of the film.
In addition, the additive can be any one of absolute ethyl alcohol or temperature raising, the pore-forming agent can be any one of polyethylene glycol (PEG) and polyvinylpyrrolidone (PVP), a desalting membrane with stable performance is obtained through the adding and dispersing effects of the additive and the pore-forming effect of the pore-forming agent, the pore-forming agent is specially selected from small molecular substances, and the purpose of forming pores is achieved through the dissolving effect of the small molecular substances.
It should be noted that the base film prepared by the invention is also modified by a modifier and finally cured by a curing agent. Generally, the addition amount of the high molecular resin powder and the N, N-dimethylacetamide is larger, the addition amount of the auxiliary materials is smaller, because if the addition amount of any component is too large, the effect of other components is covered, and the desalting effect is affected although the stability is improved, so that the compatibility relationship between the amounts is also required besides the specific matching between the formulas.
Preferably, as a further implementable aspect, the curing agent is ethyl-2-ethylacrylate.
Preferably, as a further implementable aspect, the modifying agent is a hydroxyl group-rich polymer solution.
The invention provides a formula of a desalting membrane and a preparation method thereof, and the preparation method comprises the following steps:
all the raw materials are mixed to prepare a base film, and the base film is soaked in a modifier and then is cured by a curing agent.
Preferably, as a further implementable solution, the modifier is formulated as a 5-25 wt% aqueous solution.
Preferably, as a further practicable variant, the curing agent is formulated as a 2-3% by weight aqueous solution.
The quality of the prepared desalting membrane is improved by limiting each operation parameter in the preparation method, and the desalting membrane has good stability and is suitable for COD treatment of various kinds of wastewater such as papermaking wastewater, chemical fertilizer wastewater, leather-making wastewater, metallurgical wastewater, textile wastewater, power station wastewater, coking gas wastewater, petrochemical wastewater and the like.
In a word, the desalting membrane prepared by the preparation method is green and environment-friendly and has excellent stability.
Compared with the prior art, the invention has the beneficial effects that:
(1) the desalting membrane adopts a compound formula, and multiple components are matched for use, so that the synergistic effect is obviously increased, and the desalting effect is excellent.
(2) The desalting membrane has the characteristics of simple process, lasting effect, environmental protection and the like. Is suitable for the wastewater treatment in various industries.
(3) The preparation method of the desalting membrane is simple to operate, the whole preparation method is mild in operation condition, free of pollution, free of three-waste discharge, safe and environment-friendly.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
Example 1
The specific preparation process of the desalting membrane comprises the following steps:
step one, preparation of hollow fiber desalination membrane base membrane
Weighing raw materials according to the mass fraction of 35 parts of high polymer resin powder Polysulfone (PS), 65 parts of N, N-dimethylacetamide (DMAc) solvent, 1 part of additive absolute ethyl alcohol and 10 parts of pore-forming agent polyethylene glycol (PEG), heating, dissolving and uniformly mixing in a reaction kettle, vertically entering a coagulating bath through a spinning nozzle, and obtaining the hollow fiber desalting membrane base membrane after coagulation, rinsing and soaking. The materials used for preparing the hollow fiber desalination membrane matrix are all commercial products.
Step two, preparation of low desalting membrane for COD removal
Preparing a modifier (a high molecular substance rich in hydroxyl groups) into a 25 wt% aqueous solution; curing agent 2-ethyl acrylate is prepared into 2 wt% water solution; soaking the hollow fiber desalination membrane base membrane in a modifier aqueous solution at the temperature of 30 ℃ for 8h, transferring the hollow fiber desalination membrane base membrane into a curing agent aqueous solution, heating the hollow fiber desalination membrane base membrane to 60 ℃, curing and shaping the hollow fiber desalination membrane for 120s to obtain a low desalination membrane for removing COD, and packaging, detecting and forming the product for sale.
Example 2
The specific preparation process of the desalting membrane comprises the following steps:
step one, preparation of hollow fiber desalination membrane base membrane
Weighing raw materials according to the mass fraction of 25 parts of high polymer resin powder polyether sulfone, 55 parts of N, N-dimethylacetamide (DMAc) solvent, 1 part of additive Tween and 5 parts of pore-forming agent polyvinylpyrrolidone, heating, dissolving and uniformly mixing in a reaction kettle, vertically feeding the mixture into a coagulating bath through a spinning nozzle, and obtaining the hollow fiber desalting membrane base membrane after coagulation, rinsing and soaking. The materials used for preparing the hollow fiber desalination membrane matrix are all commercial products.
Step two, preparation of low desalting membrane for COD removal
Preparing a modifier (a high molecular substance rich in hydroxyl groups) into a 5 wt% aqueous solution; curing agent 2-ethyl acrylate is prepared into 3 wt% water solution; soaking the hollow fiber desalination membrane base membrane in a modifier aqueous solution at the temperature of 30 ℃ for 8h, transferring the hollow fiber desalination membrane base membrane into a curing agent aqueous solution, heating the hollow fiber desalination membrane base membrane to 60 ℃, curing and shaping the hollow fiber desalination membrane for 120s to obtain a low desalination membrane for removing COD, and packaging, detecting and forming the product for sale.
Example 3
The specific preparation process of the desalting membrane comprises the following steps:
step one, preparation of hollow fiber desalination membrane base membrane
Weighing raw materials according to the mass fraction of 30 parts of high polymer resin powder polyether sulfone, 62 parts of N, N-dimethylacetamide (DMAc) solvent, 2 parts of additive Tween and 8 parts of pore-forming agent polyvinylpyrrolidone, heating, dissolving and uniformly mixing in a reaction kettle, vertically feeding the mixture into a coagulating bath through a spinning nozzle, and obtaining the hollow fiber desalting membrane base membrane after coagulation, rinsing and soaking. The materials used for preparing the hollow fiber desalination membrane matrix are all commercial products.
Step two, preparation of low desalting membrane for COD removal
Preparing a modifier (a high molecular substance rich in hydroxyl groups) into a 10 wt% aqueous solution; curing agent 2-ethyl acrylate is prepared into 2.5 wt% water solution; soaking the hollow fiber desalination membrane base membrane in a modifier aqueous solution at the temperature of 30 ℃ for 8h, transferring the hollow fiber desalination membrane base membrane into a curing agent aqueous solution, heating the hollow fiber desalination membrane base membrane to 60 ℃, curing and shaping the hollow fiber desalination membrane for 120s to obtain a low desalination membrane for removing COD, and packaging, detecting and forming the product for sale.
Example 4
The specific operation steps are consistent with those of the embodiment 3, only one step is adopted, and the raw materials are weighed according to the following parts by mass: the mass fraction of the high molecular resin powder polyether sulfone is 32 parts, the mass fraction of the N, N-dimethylacetamide (DMAc) solvent is 57 parts, the mass fraction of the additive Tween is 4 parts, and the mass fraction of the pore-forming agent polyvinylpyrrolidone is 6 parts.
Example 5
The specific operation steps are consistent with those of the embodiment 3, only one step is adopted, and the raw materials are weighed according to the following parts by mass: the mass fraction of the polymer resin powder polyvinylidene fluoride is 31 parts, the mass fraction of the N, N-dimethylacetamide (DMAc) solvent is 60 parts, the mass fraction of the additive Tween is 3 parts, and the mass fraction of the pore-forming agent polyvinylpyrrolidone is 7 parts.
Comparative example 1
The specific procedure is identical to example 5, except that no modifier is added.
Comparative example 2
The specific procedure was as in example 5, except that the polymeric resin powder, polyvinylidene fluoride, was 10 parts by weight and the N, N-dimethylacetamide (DMAc) solvent was 70 parts by weight.
Experimental example 1
The concrete treatment effects of the desalination films of examples 1 to 5 and comparative examples 1 to 2 were evaluated, and the concrete results are shown in the following table 1:
TABLE 1 results of treatment
As can be seen from table 1 above, the desalination membrane of the present invention has superior desalination effect compared to comparative examples 1-2, and certainly if the components are added in small amount or a component is not within the range set by the scheme of the present invention, the desalination effect is influenced to some extent, and it can be seen that each component of the scheme of the present invention is finally determined by the inventor after a great deal of practice.
In addition, as can be seen from the comparative data above, a hollow fiber desalination membrane that retains COD and allows some salt ions to permeate was obtained by the method of the present invention. The desalting rate can reach 45% at most, and the COD removal rate can reach 74% at most.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. The desalting membrane for removing COD is characterized by being mainly prepared from a base membrane, a modifier and a curing agent, wherein the base membrane is mainly prepared from the following raw materials: the composite material comprises, by mass, 25-35 parts of polymer resin powder, 55-65 parts of N, N-dimethylacetamide, 1-5 parts of an additive and 5-10 parts of a pore-forming agent.
2. The desalination membrane of claim 1, wherein the desalination membrane comprises, by mass, 30-32 parts of polymer resin powder, 57-62 parts of N, N-dimethylacetamide, 2-4 parts of an additive, and 6-8 parts of a pore-forming agent.
3. The desalination film of claim 1, wherein the desalination film comprises, by mass, 31 parts of polymer resin powder, 60 parts of N, N-dimethylacetamide, 3 parts of an additive, and 7 parts of a pore-forming agent.
4. The desalination film of claim 1, wherein the curing agent is ethyl-2-ethylacrylate.
5. The desalination membrane of claim 1, wherein the modifying agent is a hydroxyl group-rich polymer solution.
6. The desalination membrane of claim 1, wherein the polymer resin powder is any one of polysulfone, polyethersulfone or polyvinylidene fluoride.
7. The desalination membrane of claim 1, wherein the pore-forming agent is any one of polyethylene glycol and polyvinylpyrrolidone.
8. The method for preparing the desalination membrane of any one of claims 1-7, comprising the steps of:
all the raw materials are mixed to prepare a base film, and the base film is soaked in a modifier and then is cured by a curing agent.
9. The method according to claim 8, wherein the modifier is formulated in a 5-25 wt% aqueous solution.
10. The method according to claim 8, wherein the curing agent is formulated into a 2-3 wt% aqueous solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110505770.1A CN113318610A (en) | 2021-05-10 | 2021-05-10 | Desalting membrane for removing COD (chemical oxygen demand) and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110505770.1A CN113318610A (en) | 2021-05-10 | 2021-05-10 | Desalting membrane for removing COD (chemical oxygen demand) and preparation method thereof |
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| CN113318610A true CN113318610A (en) | 2021-08-31 |
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| CN202110505770.1A Pending CN113318610A (en) | 2021-05-10 | 2021-05-10 | Desalting membrane for removing COD (chemical oxygen demand) and preparation method thereof |
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| CN (1) | CN113318610A (en) |
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