CN103432995B - The renovation process of NACF in a kind of Ion exchange resin - Google Patents
The renovation process of NACF in a kind of Ion exchange resin Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 41
- 238000009418 renovation Methods 0.000 title claims abstract description 15
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000003456 ion exchange resin Substances 0.000 title claims abstract description 11
- 229920003303 ion-exchange polymer Polymers 0.000 title claims abstract description 11
- 238000011069 regeneration method Methods 0.000 claims abstract description 86
- 230000008929 regeneration Effects 0.000 claims abstract description 84
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 15
- 239000010936 titanium Substances 0.000 claims abstract description 15
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052719 titanium Inorganic materials 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 229910052742 iron Inorganic materials 0.000 claims abstract description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 45
- 230000001172 regenerating effect Effects 0.000 claims description 22
- WBZKQQHYRPRKNJ-UHFFFAOYSA-L disulfite Chemical group [O-]S(=O)S([O-])(=O)=O WBZKQQHYRPRKNJ-UHFFFAOYSA-L 0.000 claims description 13
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 12
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 4
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 3
- 229920000297 Rayon Polymers 0.000 claims description 3
- 239000004917 carbon fiber Substances 0.000 claims description 3
- 239000011148 porous material Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 229910003460 diamond Inorganic materials 0.000 claims description 2
- 239000010432 diamond Substances 0.000 claims description 2
- 230000007935 neutral effect Effects 0.000 claims description 2
- 238000012805 post-processing Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 abstract description 7
- 229910052799 carbon Inorganic materials 0.000 abstract description 5
- 230000008439 repair process Effects 0.000 abstract description 4
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 230000005684 electric field Effects 0.000 abstract description 2
- 229920006395 saturated elastomer Polymers 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 13
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 9
- 238000011049 filling Methods 0.000 description 7
- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 4
- 229910052939 potassium sulfate Inorganic materials 0.000 description 4
- 235000011151 potassium sulphates Nutrition 0.000 description 4
- 238000011084 recovery Methods 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000003575 carbonaceous material Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 230000014759 maintenance of location Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 1
- 238000011953 bioanalysis Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 238000005504 petroleum refining Methods 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000002336 sorption--desorption measurement Methods 0.000 description 1
- 230000009897 systematic effect Effects 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
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- Water Treatment By Electricity Or Magnetism (AREA)
- Water Treatment By Sorption (AREA)
Abstract
A renovation process for NACF in Ion exchange resin, the invention provides a kind of renovation process of NACF, is the renovation process for the NACF of iron in process condensate water.The method utilizes the conduction property of NACF, using NACF as anode, titanium net electrode as negative electrode, under the effect of extra electric field, make that diffusion is crossed by the Tie Tong be adsorbed on NACF, electromigration, convection current are removed from NACF, realize the regeneration of NACF.In regenerative process, add assisted Regeneration agent simultaneously, regeneration rate is further enhanced, its overall regeneration rate is more than 85%.Compared with prior art, the present invention have that regeneration rate is high, regeneration time Carbon fibe loss amount low, the feature such as energy resource consumption is little, reclaim equiment is simple.Therefore, utilize the method to regenerate the NACF of iron in process condensate water, effectively reduce Ion exchange resin cost.
Description
technical field:
The present invention relates to a kind of renovation process of NACF, be specifically related to a kind of renovation process processing the NACF of iron in condensate water.
background technology:
Steam condensate water quality is close to demineralized water, and temperature higher (being generally 90-100 DEG C), there is larger value.But carry out in petroleum refining process utilizing Steam Heating, owing to contacting with wall when steam flows in systematic pipeline, heat exchanger, the impurity such as the iron rust on wall are entrained into steam condensate, iron content in condensate water is made to exceed demineralized water index, for the consideration of saving energy and reduce the cost, reducing costs, most of chemical enterprise has the demand recycled by steam condensate.
The purification process technique of current iron content waste water mainly contains following several: (the Tang Shouyin such as oxidation-precipitation method, extraction, bioanalysis, ion-exchange, absorption method, wear friend's. waste water treatment engineering (second edition) [M]. Beijing: Chemical Industry Press, 2004,6-8.).Because absorption method is simple to operate, and do not introduce foreign ion, cost of equipment is little, the good method of a kind of deironing of can yet be regarded as.Carbonaceous material is a kind of good adsorbent, effectively can remove the various pollutants in gas phase and liquid phase.Wherein, applying maximum is active carbon, but charcoal absorption can affect the colourity of water, and powdered activated carbon not easily filters, and easily causes secondary pollution.NACF (ACF) is the new and effective activity adsorbing carbon material that 20 century 70s are developed, there is the many merits such as specific area is large, micropore is flourishing, pore-size distribution is narrow, adsorption rate is fast, adsorption capacity is large, become the sorbing material (Brasquet of most prospect of the application already, C., LeCloirec, P., Carbon, 1997,35:1307-1313.).
NACF has extraordinary adsorption/desorption performance, but expensive because of it, makes it be subject to very big restriction in actual applications.ACF production cost height is the main cause causing its price high, but is reduced costs by improvement of production process and seem near limit.Therefore, improve regeneration techniques, increasing the service life, make up the shortcoming that price is high, is effective method.（Subrenat,A.,LeCloirec,P.,Environ.Eng.,2004,130:249-257）。But some regeneration techniqueses adopted at present, also there is a lot of weak point: what disclose that " a kind of regeneration method of active carbon and regenerating active carbon system and device " adopt as CN102614855A is chemical solvent regeneration, regeneration expense is large, and the chemical solvent after regeneration deals with and quite loaded down with trivial details.In addition, though hot recycling method regeneration efficiency is high, applied range, in regenerative process must external energy heating, investment and operating cost higher, in regenerative process charcoal loss often larger; Bio-regeneration is simple, but it is long to there is the recovery time, and the impact by water quality and temperature is very large; Ultrasonic regeneration is only effective to physical absorption, and current regeneration efficiency is only about 45%, and regeneration efficiency affects larger by pore size.
summary of the invention:
Object of the present invention is exactly the deficiency existed for prior art, provides that a kind of regeneration rate is high, charcoal loss amount is low, energy resource consumption is little, the renovation process of NACF in the simple Ion exchange resin of reclaim equiment.
The technical solution used in the present invention comprises:
A renovation process for NACF in Ion exchange resin, carries out in the steps below:
1) NACF that need regenerate is as anode, and negative and positive two electrode, as negative electrode, is placed in the regeneration container filling conducting medium, adds assisted Regeneration agent, carry out pH adjustment with ammoniacal liquor by titanium net electrode.
2) connect negative electrode and anode, arranging regenerative voltage is 0.5-10V, adopts batch type, carries out regeneration process 60min-150min under uniform temperature.
3) carry out post processing cleaning with demineralized water to NACF, until water outlet is neutral, regeneration completes.
In said method step (1), NACF is viscose-based active carbon fiber felt, and its specific area is 900-2000m
2/ g, pore volume is 0.5-1.5ml/g.
In said method step (1), the titanium net of titanium net negative electrode used is characterized as: thickness of slab 0.3mm to 3mm, mesh diameter 1mm to 5mm, pass is cross mesh, hexagon ring, diamond hole etc.
In said method step (1), conducting medium is metabisulfite solution, and its concentration is 0.1mmol/L-1mmol/L.
In said method step (1), assisted Regeneration agent is citric acid, and its mass fraction is 3%-8%.
In said method step (1), ammoniacal liquor regulates pH to be 3.5-4.
In said method step (2), regeneration treatment temperature is 30-50 DEG C.
The feature of the inventive method:
1) the inventive method, utilize the conduction property of NACF, be directly anode with activated carbon fiber, titanium net electrode is negative electrode, utilize the effect of extra electric field, make that diffusion is crossed by the Tie Tong be adsorbed on NACF, electromigration, convection current are removed from NACF.
2) the inventive method improves regeneration rate using citric acid further as assisted Regeneration agent, realizes the regeneration of NACF.Citric acid has good sequestering power to metal ion, when regulating pH to be 3.5-4.0 with ammoniacal liquor, generates citric acid monoamine, now particularly outstanding to the sequestering power of iron, makes iron from ACF surface desorption.Experimental result shows, using citric acid as assisted Regeneration agent, can obtain good regeneration effect.
3) renovation process of the present invention does not need at high temperature to carry out, and reduces the energy consumption of regenerative process, decreases the loss of NACF, add the cyclic utilization rate of NACF.Thus this renovation process has very high regeneration rate, effectively reduces the cost of Ion exchange resin.
The calculating of regeneration rate:
In formula: Q is the adsorbance (mg/g) that ACF reaches when adsorbing saturation state for the first time
Q` is that after regeneration, ACF reaches the adsorbance (mg/g) when adsorbing saturation state
detailed description of the invention:
In order to better understand the present invention, below in conjunction with concrete example, the inventive method is described further, but the scope of protection of present invention is not limited to the scope that embodiment represents.
Embodiment 1 recovery time is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 4 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is 0.5mmol/L), then add 5% citric acid as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, adopt batch type to regenerate 60min, 90min, 120min, 150min, its regeneration rate is as shown in table 1:
Table 1 recovery time is on the impact of regeneration effect
| Recovery time | 60min | 90min | 120min | 150min |
| Regeneration rate | 62.8% | 77.4% | 85.7% | 86.2% |
Embodiment 2 regenerative voltage is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 4 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is 0.5mmol/L), then add 5% citric acid as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arrange regenerative voltage and be respectively 0.5V, 1.0V, 2.0V, 5V, at 30 DEG C, adopt batch type to regenerate 2 hours, its regeneration rate is as shown in table 2:
Table 2 regenerative voltage is on the impact of regeneration effect
| Regenerative voltage | 0.5V | 1.0V | 2.0V | 5.0V |
| Regeneration rate | 78.6% | 85.7% | 86.3% | 86.7% |
Embodiment 3 conducting medium metabisulfite solution concentration is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 4 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in and fill the regenerating tank that metabisulfite solution concentration is respectively 0.1mmol/L, 0.5mmol/L, 0.8mmol/L, 1.0mmol/L, add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, adopt batch type to regenerate 2 hours, its regeneration rate is as shown in table 3:
Table 3 conducting medium metabisulfite solution concentration is on the impact of regeneration effect
| Metabisulfite solution concentration | 0.1mmol/L | 0.5mmol/L | 0.8mmol/L | 1.0mmol/L |
| Regeneration rate | 79.6% | 85.7% | 77.3% | 69.7% |
Embodiment 4ACF specific area is on the impact of regeneration effect
Adopt the NACF (ACF is felted, and quality is about 0.3g, and its surface area is 25mm*25mm) of 4 kinds of different specific areas, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is respectively 0.5mmol/L), add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, adopt batch type mode to regenerate 2 hours, its regeneration rate is as shown in table 4:
Table 4ACF specific area is on the impact of regeneration effect
| ACF specific area | 900m 2/g | 1200m 2/g | 1600m 2/g | 2000m 2/g |
| Regeneration rate | 80.7% | 84.1% | 85.7% | 86.5% |
Embodiment 5 agitating mode is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 3 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is respectively 0.5mmol/L), add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, adopt different agitating mode to regenerate 2 hours, its regeneration rate is as shown in table 5:
Table 5 agitating mode is on the impact of regeneration effect
| Regeneration agitating mode | Do not stir | Stir always | Intermittent stirring |
| Regeneration rate | 74.5.% | 69.7% | 85.7% |
Embodiment 6 regeneration temperature is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 4 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, netted Ti electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is respectively 0.5mmol/L), add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, adopt batch type to regenerate 2 hours, its regeneration rate is as shown in table 6:
Table 6 regeneration temperature is on the impact of regeneration effect
| Regeneration temperature | 30℃ | 40℃ | 50℃ | 60℃ |
| Regeneration rate | 85.7% | 86.2% | 86.8% | 87.4% |
Embodiment 7 repeats the impact of regeneration times on regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, netted Ti electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in the regenerating tank filling metabisulfite solution (concentration is respectively 0.5mmol/L), add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Arranging regenerative voltage is 1.0V, adopts batch type to regenerate 2 hours at 30 DEG C.NACF is put into the solution of Fe (III) ion, until its absorption is saturated, then continue to repeat regeneration step (its regeneration condition all keeps the same at every turn), the regeneration rate after each regeneration is as shown in table 7 again:
| Regeneration times | 1st time | 2nd time | 3rd time | The 4th | The 5th |
| Regeneration rate | 85.7% | 80.2% | 79.6% | 79.2% | 79.5% |
Embodiment 8 conducting medium potassium sulfate solution concentration is on the impact of regeneration effect
Take the NACF (ACF is felted, and its surface area is 25mm*25mm) 4 parts of about 0.3g, put into the solution of Fe (III) ion, make it adsorb saturated.Using absorption saturated after ACF as anode, titanium net electrode (area is 25mm*25mm) is as negative electrode, negative and positive the two poles of the earth are placed in and fill the regenerating tank that potassium sulfate solution concentration is respectively 0.1mmol/L, 0.5mmol/L, 0.8mmol/L, 1.0mmol/L, add 5% citric acid again as assisted Regeneration agent, regulate pH value of solution to be 3.5-4.0 with ammoniacal liquor.Connect negative and positive the two poles of the earth, arranging regenerative voltage is 1.0V, and at 30 DEG C, adopt batch type to regenerate 2 hours, its regeneration rate is as shown in table 3:
Table 8 conducting medium potassium sulfate solution concentration is on the impact of regeneration effect
| Potassium sulfate solution concentration | 0.1mmol/L | 0.5mmol/L | 0.8mmol/L | 1.0mmol/L |
| Regeneration rate | 78.7% | 84.3% | 75.9% | 68.2% |
Claims (4)
1. the renovation process of NACF in Ion exchange resin, is characterized in that:
In order to regeneration viscose-based active carbon fiber felt as anode, yin, yang electrode, as negative electrode, is placed in and fills the regeneration container that conducting medium is metabisulfite solution, add assisted Regeneration agent citric acid, and add alkaline matter adjust ph by titanium net electrode; Arranging regenerative voltage is 0.5-10V, adopts batch type, carries out regeneration process, remove the iron be adsorbed on NACF under temperature is 30-50 DEG C of condition; Finally with demineralized water, post processing cleaning is carried out to NACF, until water outlet is neutral.
2. the renovation process of NACF in Ion exchange resin according to claim 1, it is characterized in that: described viscose-based active carbon fiber felt, its specific area is 900-2000m
2/ g, pore volume is 0.5-1.5ml/g; The thick 0.3-3mm of pole plate of titanium net electrode used, mesh diameter 1-5mm, pass comprises cross mesh, hexagon ring or diamond hole; Metabisulfite solution concentration is 0.1-1mmol/L; Assisted Regeneration agent citric acid mass fraction is 3-8%.
3. the renovation process of NACF in Ion exchange resin according to claim 1 and 2, is characterized in that: be the ammoniacal liquor of 25-30% in order to regulate the alkaline matter of pH.
4. the renovation process of NACF in Ion exchange resin according to claim 3, is characterized in that: regeneration treatment time is 60min-150min.
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| 重金属离子天然吸附剂的解吸和再生;黄美荣等;《化工环保》;20091231;第29卷(第5期);第385-393页 * |
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