CN103449572A - Method for simultaneously recovering dye small molecules and recycling wastewater - Google Patents
Method for simultaneously recovering dye small molecules and recycling wastewater Download PDFInfo
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- CN103449572A CN103449572A CN2013104259966A CN201310425996A CN103449572A CN 103449572 A CN103449572 A CN 103449572A CN 2013104259966 A CN2013104259966 A CN 2013104259966A CN 201310425996 A CN201310425996 A CN 201310425996A CN 103449572 A CN103449572 A CN 103449572A
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Abstract
The invention discloses a method for simultaneously recovering dye small molecules and recycling wastewater. The method comprises the following steps of step 1, selecting a charge modifier having spacer arm length, and performing charge modification on a traditional neutral ultrafiltration membrane by employing an effective chemical reaction method to obtain a charge ultrafiltration membrane with different spacer arm lengths; step 2, putting the prepared charge ultrafiltration membrane on a membrane filter, and filtering the to-be-treated water containing the dye small molecules through dead end filtration or cross flow filtration under appropriate pressure. The method provided by the invention achieves the preparation of the charge ultrafiltration membrane controllable in spacer arm length; the charge ultrafiltration membrane is capable of holding back dye small-molecule substances having the relative molecular mass from several hundred to several thousand; therefore, the dye wastewater is purified and the recycling of the dye small-molecules and the wastewater also can be realized. The method provided by the invention is simple in process, free of addition of agent, reliable in operation, compact in equipment and easy to automatically control; consequently, the membrane pollution can be effectively reduced, the service life of the membrane is prolonged and the process cost is reduced.
Description
Technical field
The present invention relates to a kind of method that simultaneously reclaims dyestuff small molecules and waste water reuse, belong to water-treatment technology field.
Background technology
Dyestuffs industries is the important industry in national economy, and its product is widely used in the fields such as textiles, leather, food, inking and rubber.China is DYE PRODUCTION big country, can produce the dyestuff of more than 550 kind of 11 large classes, and output and the volume of trade of dyestuff all rank first in the world.According to statistics synthetic dyestuff produce and treating processes in, have 12% amount to discharge with waste water formation.In all industrial sectors, the waste water of textile industry discharge is tool contaminative. the pollution caused due to the dyestuff discharge for many years is a main environmental problem always.Organic content in waste water from dyestuff is large, and great majority be take the aromatic groups such as benzene, naphthalene, anthracene, quinone and are existed as parent, have containing organic dye sewage that the water yield is large, wide, the characteristics such as change of water quality large, organic poison content is high, complicated component and difficult degradation distribute, color is very dark, colourity, up to 500～500,000, has extremely strong pollution sense, and colored water cognition affects sun exposure, be unfavorable for hydrobiological growth, general biochemical process is difficult to it is processed; Simultaneously waste water from dyestuff also has very high toxicity, is mainly to contain the organism such as halogenide, nitro thing, amino substance, aniline phenol due to some raw material and byproduct.Waste water from dyestuff is disposed to and not only pollutes in environment and endanger, especially a kind of waste of resource.Therefore, the recycling of the processing of waste water from dyestuff and dyestuff becomes problem in the urgent need to address.
Traditional dye waste water treatment method has physico-chemical process, chemical method, physisorphtion, biochemical process, electrochemical process etc., but the difficulty of governance of the current organic waste water to difficult degradation is very large, can not meet more and more higher environmental protection and processing requirement.Add more and more stricter regulation and the demand of reuse water, our active demand more economically effectively technology carry out dye wastewater treatment using.
Membrane technique because its technique is simple, energy consumption is low, do not need additionally to add medicament, reliable, facility compact and easily realize the advantage such as control automatically, be used widely in water treatment industry production in recent years, be described as " the water treatment core technology that 21 century is the most rising ".The membrane technique dye wastewater treatment using can be separated into waste water concentrated solution and see through liquid.Wherein collect concentrated solution and can realize that dyestuff reclaims, and also can be back to DYE PRODUCTION and see through liquid.Doing like this resource utilization that both can realize waste water, can not cause water pollution again, is the cleaner production important means.In water treatment procedure, several membrane techniquies commonly used mainly contain at present: reverse osmosis (RO), nanofiltration (NF), ultrafiltration (UF) and micro-filtration (MF) etc.RO and NF have good cutoff performance to the dyestuff small molecules, but the NF operating pressure is high, and energy consumption is larger.UF can effectively remove suspended particle, colloidal impurity, bacterium and germ sporangiocyst, but, with respect to the micromolecular molecular weight of dyestuff, (MWCO) is larger for the trapped molecular weight of UF film, causes it not high to the micromolecular clearance of dyestuff; Simultaneously, film pollutes the bottleneck that perplexs especially and restrict the UF application.
Through the literature search to prior art, find, open day of Chinese patent CN200810133419.9(: 2010.1.27) described the integrated technology that a kind of dyeing waste water deep purifying is processed, traditional biochemical technology is combined with ozone oxidation, air supporting, membrane sepn, can realizes the regeneration of dyeing waste water.But do not relate to the description to the ultra-filtration membrane feature in this patent, and the particle size range of the Wastewater Dyes molecule of clearly not processing.Geng Feng and Dai Haiping were delivered and have been entitled as " control that embrane method dye wastewater treatment and film pollute " literary composition in " cleaner production " the 27th the 8th phase of volume in 2005, discussed the application of embrane method in dye wastewater treatment in literary composition, in these embrane methods and have no the description to the charged ultrafiltration membrane technique with spacerarm.Mention the employing polysulphones hyperfiltration membranes such as Guo Mingyuan in article, in flat ultrafilter, the dispersed deep blue dye aqueous solution is carried out to separating experiment, find that it is feasible that polysulphones hyperfiltration membrane separates dispersed dye, but polysulfone membrane only presents faint electronegativity and can't regulate and control the charging performance power, the also particle size range of not mentioned removal dye molecule in article.In a word, there is no so far the relevant report that utilization can regulate and control the charged ultra-filtration membrane recovery small molecules dyestuff of charging performance parameter and realize waste water reclamation.
Therefore, those skilled in the art are devoted to develop the method that charged ultra-filtration membrane that a kind of utilization can regulate and control the charging performance parameter reclaims dyestuff small molecules and waste water.
Summary of the invention
In view of the shortage of prior art, technical problem to be solved by this invention is to provide a kind of method that utilization is reclaimed the dyestuff small-molecule substance with the charged ultra-filtration membrane of spacerarm simultaneously and realized waste water reuse.
For achieving the above object, the invention provides a kind of method that simultaneously reclaims dyestuff small molecules and waste water reuse, comprise the following steps:
Step 1, choose appropriate charged properties-correcting agent, and the traditional neutral ultra-filtration membrane is carried out to charged modification, obtains the charged ultra-filtration membrane of the spacerarm length of optimizing;
Step 2, be placed in described charged ultra-filtration membrane on membrane filter appts, under appropriate pressure, to containing the micromolecular waste water of dyestuff, carrying out ultrafiltration;
Described spacerarm is for connecting the hydrocarbon chain between traditional neutral ultra-filtration membrane and charged group, and spacerarm length means the number of methyl on hydrocarbon chain.
The charged ultra-filtration membrane with spacerarm that adopts charged properties-correcting agent and traditional neutral ultra-filtration membrane one step chemical reaction to make, on it, the length of spacerarm and charged properties-correcting agent is identical, and also therefore the length of spacerarm is subject to the restriction of charged properties-correcting agent.For more flexible control interval arm lengths, preferably, described charged modification divides following two steps to carry out:
The first step, the traditional neutral ultra-filtration membrane be connected intermediate reaction, spacerarm length is necessarily extended;
Second step, the traditional neutral ultra-filtration membrane that connects intermediate in grafting further reacts with described charged properties-correcting agent, the charged ultra-filtration membrane of the spacerarm length finally be optimized.
Preferably, carboxylic acid, sulfonic acid, sulfonate, ammonium salt or aminocompound that described charged properties-correcting agent is hydrocarbon chain length, structure is different.
Preferably, described bear electricity properties-correcting agent is 3-N-PROPYLE BROMIDE base sodium sulfonate, 4-bromo-butyric acid, 2-bromo acid, 2-bromotrifluoromethane sodium sulfonate, 2-chloroethyl sodium sulfonate, sodium chloroacetate, 3-chloropropionic acid, 2-methyl-3-bromo-propionic acid, 6-bromocaproic acid etc.Described lotus positive electricity properties-correcting agent is (2-bromotrifluoromethane) trimethylammonium bromide, (2-bromopropyl) trimethylammonium bromide, (3-bromopropyl) triethyl brometo de amonio, (3-carboxylic propyl group) trimethyl ammonium chloride, 2-bromine ethylamine hydrobromide etc.The reagent that extends the interval brachium is the chloro-1-hexanol of 6-, trimethylene chlorohydrin, 3-chlorine-1,2-propylene glycol, 3-glycerin chlorohydrin, the bromo-1-propyl alcohol of 3-etc.
Preferably, described traditional neutral ultra-filtration membrane is a kind of in regenerated cellulose film, cellulose acetate membrane, polyamide membrane or polyacrylonitrile film.
Preferably, described ultrafiltration adopts dead-end filtration method or cross flow filter method.
Preferably, described pressure is between 0.02-0.5MPa.
Preferably, described dyestuff small molecules is the dyestuff small molecules of reactive red, reactive brilliant bule or other lotus positive electricity or bear electricity.The particle diameter of these dye molecules is all nano levels, adopts common hyperfiltration process effectively to remove.
In the specific embodiment of the invention scheme, described charged membrane is the charged membrane with spacerarm prepared through the laboratory modification by commercial film, and adopting spacerarm length is that 9 regenerated cellulose film effects are best.
In the specific embodiment of the invention scheme, described pressure is between 0.02-0.5MPa, and the 0.02MPa effect is best.
In the specific embodiment of the invention scheme, the described ionic strength containing dyestuff small molecules water sample is between 0-10mM.
In the method that dyestuff small-molecule substance in water is removed in the present invention, can select the charged ultra-filtration membrane of different interval arm lengths, different charged groups for different dyestuff small-molecule substances, those skilled in the art can be adjusted the film parameter according to reality.
Method technique of the present invention is simple, does not need adding medicine, reliable, facility compact and easily control automatically, in the effective removal realized dye substance, can also reduce film and pollute, reduce the wash number of film, extend the work-ing life of film, reduce the cost of technology.
Embodiment
Below embodiments of the invention are elaborated: the present embodiment is implemented take technical solution of the present invention under prerequisite, provided detailed embodiment and concrete operating process, but protection scope of the present invention is not limited to following embodiment.
Embodiment 1
Step 1, prepare that pending wherein reactive red concentration is 100mg/L containing the micromolecular water sample of reactive red, regulates pH to 7.0, and ionic strength is 10mM.Choose the regenerated cellulose film that molecular weight cut-off is 30kD, its Zeta potential is-0.45mv.Adopt chemical process to carry out modification, film is immersed in sulphonic acids properties-correcting agent after 48h, the bear electricity modification regeneration cellulosic ultrafiltration membrane that to obtain spacerarm length be 3, its Zeta potential is-16.09mv.
The bear electro ultrafiltration film that step 2 is 3 by spacerarm length is placed on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.02MPa, and the ultrafiltration time is 6min.
Step 3, as a comparison, be placed in unmodified regenerated cellulose film on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.02MPa, and the ultrafiltration time is 6min.
After testing, after ultrafiltration 6min, unmodified regenerated cellulose film is 25.9% to the micromolecular clearance of reactive red; And the modification regeneration cellulose membrane of bear electricity is 88.2% to the micromolecular clearance of reactive red.More unmodified regenerated cellulose ultra-filtration membrane, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 3, improved 62.3% to the micromolecular clearance of reactive red.
Embodiment 2
Prepare that pending wherein reactive red concentration is 100mg/L containing the micromolecular water sample of reactive red, regulate pH to 7.0, ionic strength is 10mM.Choose the regenerated cellulose film that molecular weight cut-off is 30kD, its Zeta potential is-0.45mv.Adopt chemical process to carry out modification, carry out two step chemical reactions and obtain the bear electricity modification regeneration cellulosic ultrafiltration membrane that spacerarm length is 9, its Zeta potential is-25.67mv.
The bear electro ultrafiltration film that step 2 is 9 by spacerarm length is placed on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.02MPa, and the ultrafiltration time is 6min.
Step 3, as a comparison, be placed in unmodified regenerated cellulose film on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.02MPa, and the ultrafiltration time is 6min.
After testing, after ultrafiltration 6min, unmodified regenerated cellulose film is 25.9% to the micromolecular clearance of reactive red; And the modification regeneration cellulose membrane that spacerarm length is 9 bear electricity is 91.4% to the clearance of reactive red.More unmodified regenerated cellulose ultra-filtration membrane, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 9, improved 65.5% to the reactive red clearance.The modification regeneration cellulosic ultrafiltration membrane of the bear electricity that is 3 than spacerarm length, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 9, improved 3.2% to the reactive red clearance.
Embodiment 3
Step 1, prepare that pending wherein reactive brilliant bule concentration is 100mg/L containing the micromolecular water sample of reactive brilliant bule, regulates pH to 7.0.Choose the regenerated cellulose film that molecular weight cut-off is 30kD, its Zeta potential is-0.45mv.Adopt chemical process to carry out modification, film is immersed in sulphonic acids properties-correcting agent after 48h, the bear electricity modification regeneration cellulosic ultrafiltration membrane that to obtain spacerarm length be 3, its Zeta potential is-16.09mv.
The bear electro ultrafiltration film that step 2 is 3 by spacerarm length is placed on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.04MPa, and the ultrafiltration time is 6min.
Step 3, as a comparison, be placed in unmodified regenerated cellulose film on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.04MPa, and the ultrafiltration time is 6min.
After testing, after ultrafiltration 6min, unmodified regenerated cellulose film is 22.1% to the micromolecular clearance of reactive brilliant bule; And the modification regeneration cellulose membrane of bear electricity is respectively 69.8% to the micromolecular clearance of reactive brilliant bule.More unmodified regenerated cellulose ultra-filtration membrane, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 3, improved 47.7% to the micromolecular clearance of reactive brilliant bule.
Embodiment 4
Prepare that pending wherein reactive brilliant bule concentration is 100mg/L containing the micromolecular water sample of reactive brilliant bule, regulate pH to 7.0.Choose the regenerated cellulose film that molecular weight cut-off is 30kD, its Zeta potential is-0.45mv.Adopt chemical process to carry out modification, carry out two step chemical reactions and obtain the bear electricity modification regeneration cellulosic ultrafiltration membrane that spacerarm length is 9, its Zeta potential is-25.67mv.
The bear electro ultrafiltration film that step 2 is 9 by spacerarm length is placed on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.04MPa, and the ultrafiltration time is 6min.
Step 3, as a comparison, be placed in unmodified regenerated cellulose film on ultra-filtration equipment, filters pending water sample under the pressure-acting of 0.04MPa, and the ultrafiltration time is 6min.
After ultrafiltration 6min, unmodified regenerated cellulose film is 22.1% to the clearance of reactive brilliant bule; And the modification regeneration cellulose membrane that spacerarm length is 9 bear electricity is 83.4% to the clearance of reactive brilliant bule.More unmodified regenerated cellulose ultra-filtration membrane, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 9, improved 61.3% to the reactive brilliant bule clearance.The modification regeneration cellulosic ultrafiltration membrane of the bear electricity that is 3 than spacerarm length, while adopting the modification regeneration cellulosic ultrafiltration membrane filtration of the bear electricity that spacerarm length is 9, improved 13.6% to the reactive brilliant bule clearance.
The present invention, in conjunction with screening principle and charged membrane and the micromolecular electrostatic repulsion of dyestuff of ultra-filtration membrane, realizes reclaiming dyestuff small-molecule substance and waste water reuse simultaneously.Charged membrane be except utilizing screening mechanism, also can take full advantage of the electrostatic repulsion between electric charge and charged dyestuff small molecules on film and improve the micromolecular removal of dyestuff; And due to the electrocharge effect of two like magnetic poles repel each other, reduced the deposition of solute on the film surface, made the contamination resistance of film significantly increase.In the inventive method, charged ultra-filtration membrane has the incomparable advantage of traditional ultra-filtration membrane at aspects such as separation performance and contamination resistances, in water treatment field, has embodied especially the advantage that becomes increasingly conspicuous that it was increased water quality, extended membrane lifetime and reduces energy consumption.
More than describe preferred embodiment of the present invention in detail.The ordinary skill that should be appreciated that this area just can design according to the present invention be made many modifications and variations without creative work.Therefore, all technician in the art, all should be in the determined protection domain by claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (9)
1. reclaim the method for dyestuff small molecules and waste water reuse simultaneously, it is characterized in that, comprise the following steps:
Step 1, choose appropriate charged properties-correcting agent, and the traditional neutral ultra-filtration membrane is carried out to charged modification, obtains the charged ultra-filtration membrane of the spacerarm length of optimizing;
Step 2, be placed in described charged ultra-filtration membrane on membrane filter appts, under appropriate pressure, to containing the micromolecular waste water of dyestuff, carrying out ultrafiltration;
Described spacerarm is for connecting the hydrocarbon chain between traditional neutral ultra-filtration membrane and charged group, and spacerarm length means the number of methyl on hydrocarbon chain.
2. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said charged modification divides following two steps to carry out:
The first step, the traditional neutral ultra-filtration membrane be connected intermediate reaction, spacerarm length is necessarily extended;
Second step, the traditional neutral ultra-filtration membrane that connects intermediate in grafting further reacts with described charged properties-correcting agent, the charged ultra-filtration membrane of the spacerarm length finally be optimized.
3. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said charged properties-correcting agent is carboxylic acid, sulfonic acid, sulfonate, ammonium salt or aminocompound.
4. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said bear electricity properties-correcting agent is 3-N-PROPYLE BROMIDE base sodium sulfonate, 4-bromo-butyric acid, 2-bromo acid, 2-bromotrifluoromethane sodium sulfonate, 2-chloroethyl sodium sulfonate, sodium chloroacetate, 3-chloropropionic acid, 2-methyl-3-bromo-propionic acid, 6-bromocaproic acid etc.Wherein said lotus positive electricity properties-correcting agent is (2-bromotrifluoromethane) trimethylammonium bromide, (2-bromopropyl) trimethylammonium bromide, (3-bromopropyl) triethyl brometo de amonio, (3-carboxylic propyl group) trimethyl ammonium chloride, 2-bromine ethylamine hydrobromide etc.The reagent that extends the interval brachium is the chloro-1-hexanol of 6-, trimethylene chlorohydrin, 3-chlorine-1,2-propylene glycol, 3-glycerin chlorohydrin, the bromo-1-propyl alcohol of 3-etc.
5. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said traditional neutral ultra-filtration membrane is a kind of in regenerated cellulose film, cellulose acetate membrane, polyamide membrane or polyacrylonitrile film.
6. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said ultrafiltration adopts the dead-end filtration method.
7. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said ultrafiltration adopts the cross flow filter method.
8. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said pressure is between 0.02-0.5MPa.
9. the method that simultaneously reclaims dyestuff small molecules and waste water reuse as claimed in claim 1, wherein said dyestuff small molecules is reactive red or reactive brilliant bule.
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| CN101555048A (en) * | 2009-05-21 | 2009-10-14 | 上海交通大学 | Method for removing natural organism and heavy metal simultaneously from water |
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2013
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| US4412922A (en) * | 1980-07-02 | 1983-11-01 | Abcor, Inc. | Positive-charged ultrafiltration membrane for the separation of cathodic/electrodeposition-paint compositions |
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| US20020185440A1 (en) * | 2001-02-02 | 2002-12-12 | Eastman Kodak Company | Method for recycling wash-water resulting from film treatment |
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Application publication date: 20131218 |