CN101298058A - Modified cation-exchange resin and preparation and use thereof - Google Patents
Modified cation-exchange resin and preparation and use thereof Download PDFInfo
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- CN101298058A CN101298058A CNA2008100389048A CN200810038904A CN101298058A CN 101298058 A CN101298058 A CN 101298058A CN A2008100389048 A CNA2008100389048 A CN A2008100389048A CN 200810038904 A CN200810038904 A CN 200810038904A CN 101298058 A CN101298058 A CN 101298058A
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Abstract
The invention discloses a modified cation exchange resin and a preparation method and an application thereof. The modified cation exchange resin of the invention has relatively good effect on processing oily waste water and has an oil removal rate up to over 80 percent and turbidity removal rate up to over 60 percent by test. In addition, the preparation method and process technique are simple and do not need any chemical agent, thus having low operation cost; meanwhile, oil in the waste water after being processed can be recycled, thus avoiding secondary pollution and high energy consumption.
Description
Technical field
The present invention relates to a kind of modified cation-exchange resin and its production and application.
Background technology
Oily waste water is the big and wide pollution sources of a kind of amount, show according to interrelated data, have at least every year ten thousand tons of oils of 500-1000 to enter water body by all means in the world, have a strong impact on the use value of water resource, serious pollution and destruction are also caused in biosphere, atmospheric thermodynamics etc., be detrimental to health and living environment.The oily waste water main source has following several: (1) oil exploitation processing; (2) petrochemical industry; (3) metallurgy; (4) mechanical industry; (5) other sources are divided by outside the last source, and industry such as grain and oil processing for another example, leather, papermaking, weaving, food also have a large amount of oil-polluted water dischargings.
Oily substance swims in water surface formation thin film and can stop airborne oxygen to be dissolved in the water, dissolved oxygen in the water is reduced cause in the water body planktonic organism etc. dead because of anoxic, thereby the photosynthesis that has also hindered water plant influences the self purification of water body, even makes the water quality fouling destroy the value of water resource.Some noxious materials in oil and the catabolite thereof (as BaP, benzanthracene and other polycyclic aromatic hydrocarbon) are lower to the lethasl concentration of various biologies.On the one hand, direct toxic action takes place to biology in these noxious materials, on the other hand, the water that contains micro oil that is lower than lethasl concentration be used for culturing or when irrigating by bio-absorbable and enrichment, entering human body by food chain then is detrimental to health, contain other metal ion of iron copper and bacterium etc. in the sewage simultaneously, they can play the media facilitation, and the special decomposition that can accelerate sump oil in the waste water of high temperature is gone bad.A small amount of sulfur oxide of soda water is the end product of petroleum oxidation, thereby the aeration condition of water body is degenerated, and influences hydrobiological normal growth, even causes the death of animals and plants colony.If be used for irrigating, when surpassing, the composition of oil allows content, and then stop up soil and cause crop failure or necrosis, make fruit have the oil flavor, if permeate the ground then polluted underground water.So it is current urgent problem that oily waste water is administered, significant to human survival and social sustainable development.
Many in the world countries have all done regulation and restriction to the oil concentration of waste discharge.China has issued all kinds of environmental quality standards, and wherein " integrated wastewater discharge standard " (GB8978-1996) proposed very high requirement at the petroleum-type pollutant.The pollutant discharging unit that national regulation was built after 1 day January in 1998, the primary standard of the highest permission concentration of emission of petroleum-type pollutant is 5mg/L.
In recent years, the stakeholder has carried out the theory and practice exploration with regard to the effect that how further to improve oil processing in the industry.Oil content in the oily water exists with the state of suspended oil, dispersed oil, oil emulsion, dissolved oil, according to the existence of oil, can carry out classification to oily waste water and handle.In petrochemical enterprise, oil extraction process and place such as metal cutting produce emulsifiable oil waste water because its state is more stable, handle difficulty.So find a kind of technology simple, effect is obvious, cost is not high, and can make disposes of sewage reaches the requirement of discharging, reaches the new technology of recovered oil simultaneously again, becomes the problem that people pay close attention to.
Summary of the invention
Technical problem to be solved by this invention is relatively poor in order to overcome when handling oily waste water the traditional treatment method effect, cost is higher, the difficult defective that reaches emission request of disposing of sewage, and a kind of modified cation-exchange resin and its production and application is disclosed.Modified cation-exchange resin preparation method of the present invention is simple, and it is used for oily waste water handles, and treatment process is simple, and effect is obvious, does not need to add any chemical agent, and operating cost is low, and the while can be reclaimed the oil after the wastewater treatment again.
Modified cation-exchange resin of the present invention is connected to cetyl trimethyl quaternary ammonium cation group.The quantity of described cetyl trimethyl quaternary ammonium cation account for this modified cation-exchange resin the exchangeable cations total quantity 10%～90%, what be more preferably is 30～65%.
The invention still further relates to the preparation method of modified cation-exchange resin of the present invention, it comprises the following steps: a kind of cationic ion-exchange resin is immersed in the solution of softex kw (CTAB), heating and isothermal reaction can obtain modified cation-exchange resin of the present invention.
Wherein, the concentration of the aqueous solution of described softex kw is preferable 25～60g/L when being 60 ℃, that better is 60g/L.The mole that is in excess in exchangeable cations on the cationic ion-exchange resin that the consumption of described softex kw is preferable is preferably 1.1～1.5 times of mole of exchangeable cations on the cationic ion-exchange resin, and better is 1.2 times.
Wherein, described be heated to the temperature of constant temperature preferable be 60～70 ℃, better is 70 ℃.Water-bath adopted that mode of heating is preferable or oil bath.What described reaction was preferable carries out under vibration, and what the time of vibration was preferable is 4～6 hours.The instrument that vibrates can be constant temperature oscillator, and what its rotating speed was preferable is 100～200/ minutes.After reaction finishes, be cooled to room temperature, the water flushing, get final product modified cation-exchange resin of the present invention.What wherein, described water was preferable is deionized water.
Wherein, described cationic ion-exchange resin can be selected the existing various cationic ion-exchange resins in this area for use.From contained cation group, mainly comprise storng-acid cation exchange resin and weak-acid cation-exchange resin, preferred storng-acid cation exchange resin, as contain sulfonic group (SO
3H) storng-acid cation exchange resin.The cationic ion-exchange resin of other ionic species that are transformed into by above-mentioned highly acid or weak-acid cation-exchange resin as the sodium type, also is applicable to the present invention.From pore structure, gel-type and macroporous type all are applicable to the present invention.From the matrix of ion exchange resin, existing various substrates all are applicable to the present invention as polystyrene, acrylic acid or acrylic ester, phenolic aldehyde system (FP) etc., optimization styrene system.Among the present invention, the preferred cation exchanger resin is strongly acidic styrene type cation exchange resin HZ016, gel-type strongly acidic styrene type cation exchange resin JK006 or macroporous type strongly acidic styrene type cation exchange resin D001.
Described cationic ion-exchange resin can use the commercial goods, also can make by oneself by this area conventional method.For example, sulfonated polystyrene type resin can be prepared by following method: with styrene is monomer, divinylbenzene is a crosslinking agent, under dibenzoyl peroxide catalysis, carry out copolyreaction, make polystyrene resin, adopt concentrated acid sulfonation to introduce the hydrophily sulfonic acid group again, can make, reaction scheme is as follows:
When adopting commercially available resin cationic ion-exchange resin commodity of buying, preferable carry out preliminary treatment earlier, to remove impurity, improve the grafting amount of cetyl trimethyl quaternary ammonium cation in the modifying process, concrete steps as: sieve, washing, after removing a small amount of organic matter of absorption with alcohol immersion again, soak with saturated aqueous common salt, use the HCl and the NaOH solution (the preferred 1.0mol/L of the concentration of bronsted lowry acids and bases bronsted lowry solution) of 8～10 times of volumes again, according to the sequence alternate washing by soaking of soda acid acid, make it change into the H type, be washed till neutrality with deionized water at last.
The mechanism that the present invention carries out cationic ion-exchange resin remodeling replaces with cetyl trimethyl quaternary ammonium cation group for the cation with used cationic ion-exchange resin.Storng-acid cation exchange resin with band sulfonic group or sodium sulfonate group is an example, and it is as follows to provide reaction equation:
Wherein, y＞x, R are the cationic ion-exchange resin substrate.
The present invention also further relates to the application of modified cation-exchange resin of the present invention in handling oily waste water.
Concrete operations can be carried out as follows: with the oily waste water modified cation-exchange resin layer of the present invention of flowing through from bottom to top, discharge from the upper end outlet, will discharge liquid and leave standstill, it can be divided into the profit two-phase, oil phase is removed or collection gets final product.Wherein, modified cation-exchange resin of the present invention can be filled in glass tube or the stainless steel tube.That bore is preferable is 2cm; What the diameter aspect ratio of glass tube was preferable is 1: 10～1: 15; That the air speed of described wastewater treatment is preferable is 1.0～6.0h
-1What operating temperature was preferable is 20～45 ℃.
Adopt existing blank resin (as common styrene resin) to handle oily waste water,, can only rely on the oil in the physical adsorption way absorption removal oily waste water because it does not have hydrophilic and hydrophobic grouping.After the hole on resin particle surface was covered by oil, the effect of oil removing will descend.
Modified cation-exchange resin of the present invention is then different with it, and it is by adsorbing the coalescent demulsification that reaches.The cetyl trimethyl quaternary ammonium cation group that is connect on the modified cation-exchange resin of the present invention has lipophile preferably, also have on the resin in addition partially modified before contained hydrophily cation itself (as-SO
3H).When oily waste water passed through the modified resin bed, the chain alkyl of the cetyl trimethyl quaternary ammonium cation group of oleophylic can adsorb little oil droplet.Simultaneously, also the neutralized part negative electrical charge of the medium and small oil droplets of waste water of positively charged cetyl trimethyl quaternary ammonium cation group has compressed the electric double layer of oil droplet, makes zeta current potential absolute value descend significantly, each other repulsive force descends between the oil droplet, is easier to be adsorbed on the resin particle; Along with constantly carrying out of adsorption process, micron-sized oil droplet constantly in the resin surface cohesion, forms oil film adsorption layer closely.After this, the increase of oil film thickness makes the cross-sectional area of water stream channel diminish.Under the constant situation of flow, it is big that water velocity becomes.The resin of the water collision coalescence oil droplet that flows has increased the frictional force between current and the oil film, makes oil film move up under the drive of current.Oil film runs into the hydrophilic radical on the resin in the process that moves up, oil film distortion and from the resin desorption get off, form the bulky grain come-up, thereby the oil droplet in the waste water removed, and finish the automatic regeneration of resin.In addition, the repulsive force between the little oil droplet that is not adsorbed is because the minimizing of the carried charge on surface can aggregate into the larger oil droplet come-up, emulsion stability decreases, thereby and aqueous phase separation gradually.
The present invention is raw materials used and reagent is all commercially available gets.
Positive progressive effect of the present invention is: modified cation-exchange resin of the present invention has preferable oily waste water treatment effect, after tested, can reach more than 80% oil removing rate in the oily waste water, and turbidity removal rate can reach more than 60%.And its preparation method is simple, and treatment process is simple, does not need to add any chemical agent, and operating cost is low, and the while can also be reclaimed the oil after the wastewater treatment, avoids secondary pollution and high energy consumption.
Description of drawings
Fig. 1 carries out the process chart that oily waste water is handled for adopting modified cation-exchange resin of the present invention.Wherein, 1 is agitator, and 2 is the oily waste water intake chamber, and 3 is peristaltic pump, and 4 is a resin packed layer, and 5 is No. two resin packed layers, and 6 is effluent trough.
Oily waste water is through stirring, and entered in the middle of the resin packed column by peristaltic pump, and what resin packed layer used is not have modified resins, and what No. two resin packed layers used is the resin of modification, and the water outlet after the processing enters in the effluent trough.
Fig. 2 is the coarse schematic representation of apparatus of potting resin in the technological process of oily waste water processing.
Waste water adopts up flow type to enter in the resin column by peristaltic pump, and the bottom of resin column is a uniform board, is used for fixing resin and distribution current, and anti-resin particle sedimentation enters in the inlet channel.It is fixing that resin bed top uses stainless steel wire to fill.The glass tube the top is a delivery port.
The specific embodiment
Further specify the present invention with embodiment below, but the present invention is not limited.
Select for use through pretreated D001 resin, make reaction dissolvent with deionized water, ethanol, isopropyl alcohol respectively, under 25 ℃, 50 ℃, 60 ℃ and 70 ℃, exchange graft reaction respectively and carry out modification.Reagent dosage is the 1gCTAB/10g wet resin, the 30mL solvent.
The utilization ratio of grafting efficiency percentage: ctab (GE) promptly refers to participate in reaction and finally is grafted to the ratio that CTAB quality on the resin accounts for total adding quality, embodies the influence of different solvents different temperatures to reaction.
The result shows, under the situation of 25 ℃ of room temperatures, because the solubility of CTAB in alcohols is higher than its solubility in water, the grafting efficiency difference in the different solutions is obvious, grafting efficiency in ethanol and isopropyl alcohol is respectively 59% and 57%, and the efficient in water is 41%.The Kraft point of CTAB is about 30 ℃, and when temperature surpassed this temperature, the solubility of ionic surfactant in water significantly rose.And the rising temperature helps the carrying out of exchange reaction.Along with temperature rises, the grafting efficiency of CTAB in deionized water improves very fast, and when temperature was 60 ℃, efficient had reached 94%.Reacted down lasting 4 hours at 60 ℃, can prepare good modified resin.
The clearance of effect embodiment 1 turbidity and oil
(gel-type strongly acidic styrene type cation exchange resin JK006 (every gram resin wet basis CEC is 2.4mmol) is at 60 ℃ to get the modified resin of 25ml respectively, isothermal vibration reaction 6h in the CTAB aqueous solution of 50g/L, rotating speed is 100r/min, the grafting amount is that (the JK006 resin is processed into Hydrogen with the hydrochloric acid of 1mol/L, and case 1 and 2 is all made of these two resins for 0.39gCTAB/g resin (sulfonic acid group utilization rate 45%) and unmodified resin.) fill out post, be that 20 ℃, flow velocity are under the condition of 15ml/min in water temperature, the emulsified oil-containing waste water that the oil concentration and the turbidity of water inlet is respectively 329.3mg/L and 474NTU is handled, take out water gaging turbidity and oil content behind the operation 1h.The removal effect of the turbidity of two pillars and oil sees Table 1.
Can find that by table 1 oil content and the turbidity of modified resin R-CTAB and the water outlet of unmodified resin R-H pillar are all variant.The oil content of R-H pillar water outlet is 68.2mg/L, and turbidity is 260NTU, and the oil content of R-CTAB pillar water outlet and turbidity are respectively 47.4mg/L and 215NTU, and is all low than the water outlet of R-H pillar; The oil removing rate of R-CTAB pillar and turbidity removal rate are respectively 85.6% and 54.6%, than the clearance difference high 6.3% and 9.5% of R-H pillar.Resin oil removing after the modification is described and go turbid effect all to be better than unmodified.This mainly is that mainly by resin adsorption, after the hole on resin particle surface was covered by oil, the effect of oil removing will descend because during unmodified resin coalesced oil removing.And the modified resin surface has the lipophilic group of long-chain, and lipophile strengthens, so deoiling effect is good.
Table 1 R-H and R-CTAB are to the removal effect of oil and turbidity
| Oil content/(mg L -1) | Turbidity/(NTU) | Oil removing rate/(%) | Turbidity removal rate/(%) | |
| Water inlet | 329.3 | 474 | / | / |
| The R-H water outlet | 68.2 | 260 | 79.3 | 45.1 |
| The R-CTAB water outlet | 47.4 | 215 | 85.6 | 54.6 |
| R-CTAB and R-H water outlet difference | -20.8 | -45 | 6.3 | 9.5 |
The influence of 2 pairs of waste water Zeta potentials of effect embodiment
25 ℃ of water temperatures, pH is 7.6, the emulsifying agent mass concentration is under 0.01% the situation, the zeta potential value of oily waste water is-54.48mv, the tiny oil droplets surface that disperses in the waste water has more negative electrical charge, cause oil droplet to repel mutually and be difficult for contact and coalescent, oily waste water system gross energy is very low, keeps stable state to be difficult to automatic coalescent layering.After two filled columns processing through two modifications and unmodified resin, the zeta potential value of oil droplet all decreases in the waste water.In the operation phase, the zeta current potential mean value of modified resin post water outlet is-20.9mv that the zeta current potential mean value of unmodified resin post water outlet is-37.6mv that zeta current potential absolute value has reduced by 61.6% and 31.0% respectively before handling.Because the cationic effect of CTAB, oil droplet zeta current potential absolute value declines to a great extent in the waste water, has reduced the stability of system, help emulsion drop coalescent each other take off steady.And the electrostatic attraction between cation and the electronegative oil droplet, obviously do not subdue the stability that influences oil droplet that can be long-term along with time lengthening.
The oil concentration of effect embodiment 3 oily waste waters is to the influence of treatment effect
Used resin: large hole strong acid styrene system cation exchange resin D001 (the wet basis CEC is 1.7mmol) is at 60 ℃, isothermal vibration reaction 6h in the CTAB aqueous solution of 50g/L, rotating speed is 120r/min, and the grafting amount is 0.28gCTAB/g resin (a sulfonic acid group utilization rate 45%).
Get the waste water A and the B of variable concentrations, oil content is respectively 177.5mg/L and 307.1mg/L, and corresponding turbidity is 205NITU and 314NTU, is 1.8h in liquid air speed
-1, water temperature is under 20 ℃ of conditions, through 300cm
3The modified resin filled column is handled.Oil removing rate and turbidity removal rate see Table 2.
The concentration of table 2 water inlet is to the influence of oil and turbidity removal rate
As can be seen from Table 2, two kinds of different waste water of water inlet initial concentration are under the condition of the identical water temperature of identical flow velocity, through identical resin extender post, treatment effect difference.Water inlet contains the high waste water of oil emulsion oil mass, and before initial 3 hours, because mass transfer force is big, the B sample is than the clearance high 5.42% and 11.41% of A sample to oil and turbidity.But along with the prolongation in processing time and the increase of wastewater treatment capacity, both difference is dwindled gradually.After having moved 6h continuously, modified resin is basicly stable about 80% and 50% to the oil and the turbidity removal rate of A, B two water samples.
Claims (9)
1, a kind of modified cation-exchange resin is characterized in that: it is connected to cetyl trimethyl quaternary ammonium cation group.
2, modified cation-exchange resin as claimed in claim 1 is characterized in that: the quantity of described cetyl trimethyl quaternary ammonium cation account for this modified cation-exchange resin the exchangeable cations total quantity 10%～90%.
3, modified cation-exchange resin as claimed in claim 2 is characterized in that: the quantity of described cetyl trimethyl quaternary ammonium cation account for this modified cation-exchange resin the exchangeable cations total quantity 30～65%.
4, the preparation method of modified cation-exchange resin as claimed in claim 1, it comprises the following steps: a kind of cationic ion-exchange resin is immersed in the solution of softex kw, and heating and isothermal reaction get final product.
5, method as claimed in claim 4 is characterized in that: 25～60g/L when the concentration of the aqueous solution of described softex kw is 60 ℃.
6, method as claimed in claim 4 is characterized in that: the consumption of described softex kw is 1.1～1.5 times of mole of exchangeable cations on the cationic ion-exchange resin.
7, method as claimed in claim 4 is characterized in that: the described temperature that is heated to constant temperature is 60～70 ℃.
8, method as claimed in claim 4 is characterized in that: described cationic ion-exchange resin is storng-acid cation exchange resin or property sodium type cationic ion-exchange resin.
9, method as claimed in claim 4 is characterized in that: described cationic ion-exchange resin is strongly acidic styrene type cation exchange resin HZ016, gel-type strongly acidic styrene type cation exchange resin JK006 or macroporous type strongly acidic styrene type cation exchange resin D001.
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| CN110773115A (en) * | 2019-11-20 | 2020-02-11 | 苏州溪能环保科技有限公司 | High-efficient water treatment facilities |
| CN110773115B (en) * | 2019-11-20 | 2022-07-12 | 苏州溪能环保科技有限公司 | High-efficiency water treatment device |
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