CN1559922A - Process for adsorpting and separating waste water containing nitro-chlrobenzene by antimony oxide modified zeloite and resource recovery process thereof - Google Patents
Process for adsorpting and separating waste water containing nitro-chlrobenzene by antimony oxide modified zeloite and resource recovery process thereof Download PDFInfo
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- CN1559922A CN1559922A CNA2004100142583A CN200410014258A CN1559922A CN 1559922 A CN1559922 A CN 1559922A CN A2004100142583 A CNA2004100142583 A CN A2004100142583A CN 200410014258 A CN200410014258 A CN 200410014258A CN 1559922 A CN1559922 A CN 1559922A
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- zeolite
- hzsm
- waste water
- nitro
- weisspiessglanz
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- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000002351 wastewater Substances 0.000 title claims abstract description 14
- 238000011084 recovery Methods 0.000 title description 10
- 229910000410 antimony oxide Inorganic materials 0.000 title 1
- VTRUBDSFZJNXHI-UHFFFAOYSA-N oxoantimony Chemical compound [Sb]=O VTRUBDSFZJNXHI-UHFFFAOYSA-N 0.000 title 1
- BFCFYVKQTRLZHA-UHFFFAOYSA-N 1-chloro-2-nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1Cl BFCFYVKQTRLZHA-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 41
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 41
- 239000010457 zeolite Substances 0.000 claims abstract description 41
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000010815 organic waste Substances 0.000 claims abstract description 10
- GHPGOEFPKIHBNM-UHFFFAOYSA-N antimony(3+);oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Sb+3].[Sb+3] GHPGOEFPKIHBNM-UHFFFAOYSA-N 0.000 claims description 26
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 238000001354 calcination Methods 0.000 claims description 7
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- 238000013019 agitation Methods 0.000 claims description 2
- 239000011812 mixed powder Substances 0.000 claims description 2
- 238000002203 pretreatment Methods 0.000 claims description 2
- 238000004064 recycling Methods 0.000 claims description 2
- 238000007789 sealing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims 2
- 239000003795 chemical substances by application Substances 0.000 claims 1
- 239000003960 organic solvent Substances 0.000 claims 1
- 239000000843 powder Substances 0.000 abstract description 4
- 238000003746 solid phase reaction Methods 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 abstract description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 abstract 2
- 150000005181 nitrobenzenes Chemical class 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 description 18
- 238000010521 absorption reaction Methods 0.000 description 6
- 239000002808 molecular sieve Substances 0.000 description 6
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- 239000003463 adsorbent Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 238000005194 fractionation Methods 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000007787 solid Substances 0.000 description 3
- 238000010671 solid-state reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- MVPPADPHJFYWMZ-UHFFFAOYSA-N chlorobenzene Chemical compound ClC1=CC=CC=C1 MVPPADPHJFYWMZ-UHFFFAOYSA-N 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000002594 sorbent Substances 0.000 description 2
- 229910004283 SiO 4 Inorganic materials 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002414 normal-phase solid-phase extraction Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- -1 silicon aluminate Chemical class 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention is a method of using stibium oxide decorated HZSM-5 zeolite to absorb and separate nitrobenzene organic waste water and recovering resources, transporting the organic waste water containing nitrobenzene isomer to be processed to an absorbing container holding the stibium oxide decorated HZSM-5 zeolite for absorbing. The particle size of the HZSM-5 zeolite is 0.5-20 mum; the stibium oxide accounts for 5%-20% of the mass of the powder before burned; the initial concentration ratio of ortho-isomer to para-isomer of nitrochlorobenzene in the waste water is 1-5 to 1; the vibrating speed is 50-200 r/min; the temperature range is 275-340 K; the absorbing time is 10 s-12 h. It utilizes the character that the special crystal structure of HZSM-5 zeolite and the solid-phase reaction of HZSM-5 zeolite with the stibium oxide powder cause the variation of surface structure of the HZSM-5 zeolite, to efficiently separate ortho-nitrochlorobenzene and para-nitrochlorobenzene from the nitrochlorobenzene waste water, respectively.
Description
Technical field
The present invention relates to a kind of method of from the organic waste water that contains the nitro-chlorobenzene isomer, selecting the fractionation by adsorption nitro-chlorobenzene, the method for particularly a kind of HZSM-5 zeolite of modifying with weisspiessglanz fractionation by adsorption p-Nitrophenyl chloride and o-Nitrochlorobenzene from the waste water that contains the nitro-chlorobenzene isomers.
Background technology
Absorption is a kind of Solid-Phase Extraction isolation technique of less energy-consumption.Adsorption be since the molecule of solid surface or atom because of discontinuity equalization has remaining surface energy.When some materials collision solid surface, be subjected to the attraction of these unbalanced forces and be trapped on the solid surface, make be adsorbed molecule adsorbent surface concentration be higher than the solution body mutually in concentration.Handle the sorbent material that meticulous organic chemical waste water mainly adopts with absorption method gac and resin etc. are arranged.The charcoal absorption performance is preferable, but its regeneration difficulty, the material of absorption is difficult to realize resource utilization.Polymeric adsorbent is applied and forms a kind of adsorption separation technology of uniqueness in every field.But existing resin choice is not high, and is also very difficult for effective separation of close organism isomer of character or homologue.
Zeolite is a kind of many micropores silicon aluminate crystal of moisture shape structure, is by silica (SiO
4) tetrahedron and alumina (AlO
4) tetrahedron element is staggered to spacial framework by the Sauerstoffatom that is in tetrahedron top.Exist a large amount of holes in crystalline structure, movably water molecules and positively charged ion are distributing in the hole.This constructional feature makes zeolite have absorption, catalysis and the ion-exchange three big characteristics of selection.HZSM-5 has the pore canal system that 3 D stereo intersects, and channel diameter is respectively 0.51 * 0.55nm, 0.53 * 0.56nm, and these two kinds of dissimilar ducts diameter of the vertical intersection point that forms mutually are 0.89nm.Owing to its uniform micropore size and benzene molecular sizableness, formed the selection characterization of adsorption of molecular sieve thus, promptly have only molecule suitable or ion just can enter zeolite cavity with zeolite pore.In the isomers of nitro-chlorobenzene, the critical kinetic diameter of para-isomeride is suitable with the channel diameter of HZSM-5 zeolite, and ortho position and meta-isomer are big than the channel diameter of HZSM-5 zeolite, like this because the current drag effect in duct, make the less para-isomeride of molecule critical diameter than and ortho position and meta-isomer are easier to be diffused in the hole in and be adsorbed, thereby show para-isomeride is had the performance that selection is adsorbed.
By the outside surface of HZSM-5 zeolite being modified the aperture size that can reduce molecular sieve effectively, thereby further improve the selective adsorption performance of molecular sieve.One of present research focus is that zeolite surface is carried out modification and modification, common modifying method has chemical vapors (or liquid phase) deposition and metal oxide solid state reaction etc., but the sign of the zeolite molecular sieve after technology of preparing, modification and stable aspect still need do a large amount of work.Weisspiessglanz can be dispersed in the HZSM-5 zeolite surface by the hydroxyl generation solid state reaction with the HZSM-5 zeolite surface uniform high-efficiency, causes HZSM-5 zeolite aperture to narrow down.
Summary of the invention
The present invention seeks at the deficiencies in the prior art, a kind of adsorption separation technology of high-efficiency low energy consumption is provided, the selection adsorption of the HZSM-5 zeolite of modifying by weisspiessglanz separates from the organic waste water that contains the close nitro-chlorobenzene isomer of character and reclaims p-Nitrophenyl chloride and o-Nitrochlorobenzene.
Technical scheme of the present invention:
The HZSM-5 zeolite adsorption that a kind of weisspiessglanz is modified is separated and is contained nitro-chlorobenzene waste water and resource recycling method, it is characterized in that the organic waste water that contains the nitro-chlorobenzene isomer that will handle is delivered to the contactor that the HZSM-5 zeolite that weisspiessglanz modifies is housed and adsorbs, its condition is: the HZSM-5 zeolite granular diameter that weisspiessglanz is modified is 0.5～20 μ m; Weisspiessglanz accounts for 5%～20% of the preceding mixed powder quality of calcining; Nitro-chlorobenzene ortho isomer and the para-isomeride starting point concentration ratio in waste water is 1～5: 1; The vibration rotating speed is 50～200 rev/mins; Temperature range is 275～340K; Adsorption time is 10s～12h.
Beneficial effect of the present invention:
The present invention compared with prior art, its remarkable advantage is: present method is utilized the pore passage structure of HZSM-5 zeolite uniqueness and HZSM-5 zeolite and weisspiessglanz powder generation solid state reaction and is caused the characteristics of HZSM-5 zeolite surface structural changes, isolates p-Nitrophenyl chloride and o-Nitrochlorobenzene in the nitro-chlorobenzene waste water efficiently.The separating effect of nitro-chlorobenzene isomer is relevant with HZSM-5 zeolite surface structure, and the HZSM-5 zeolite that weisspiessglanz is modified improves the separating effect of nitro-chlorobenzene isomer because of the aperture narrows down.So can improve selection absorption property to para-isomeride by the HZSM-5 zeolite after the weisspiessglanz modification.
When the present invention is used to handle the organic waste water that contains the nitro-chlorobenzene isomer, the rate of recovery of p-Nitrophenyl chloride and o-Nitrochlorobenzene can be respectively up to more than 99.5% and 95%, efficient low-consume has been realized the resource utilization of waste water, has overcome the defective that gac and polymeric adsorbent are handled waste water.Simultaneously, the HZSM-5 zeolite be a kind of nontoxic, tasteless, environment is not had the sorbent material of influence, and fabulous acid resistance, thermostability and water vapour stability are arranged, molecular sieve can use repeatedly simultaneously.Therefore, the present invention is used to handle organic waste water and has good economic benefit and environmental benefit, has very wide application prospect.
Embodiment
Below further specify the present invention by example.
Embodiment 1: the organic waste water of the nitrated generation of HZSM-5 zeolite treatment chlorobenzene of modifying with weisspiessglanz.
Weisspiessglanz and HZSM-5 zeolite powder are mixed by the quality proportioning at 1: 4, at N
2Protection under be warming up to 500 ℃ with the speed of 10 ℃/min, and at this temperature lower calcination 2h.Get organic waste water 400ml, wherein the p-Nitrophenyl chloride starting point concentration is 25mg/L, and waste water is carried out some conventional pre-treatment, as filtering, regulate pH value etc.The total mass of HZSM-5 zeolite and weisspiessglanz mixture is 0.17g before modifying, and weisspiessglanz accounts for 20% of the preceding mixture total mass of calcining, is about 0.034g.The HZSM-5 zeolite Si/Al that modifies with weisspiessglanz is 48; The HZSM-5 zeolite granular diameter of modifying with weisspiessglanz is 5 μ m; The contactor sealing; Adopt magnetic agitation, the vibration rotating speed is 150 rev/mins; The o-Nitrochlorobenzene starting point concentration: the p-Nitrophenyl chloride starting point concentration is 1: 1; Temperature is got 300K; Adsorption time is 60min.The p-Nitrophenyl chloride separation rate reaches 99.2%, and the separation rate of o-Nitrochlorobenzene is 95.1% (separation rate is meant after the molecular sieve property selected fractionation by adsorption, the content of nitro-chlorobenzene in each separated portion).Adopt ethanol as reclaiming liquid, the rate of recovery of nitro-chlorobenzene is 99.5% when 300K.
Embodiment 2: among the embodiment 1, other condition is constant, and when adsorption time was 5min, the separation rate of p-Nitrophenyl chloride was up to 99.8%, and the separation rate of o-Nitrochlorobenzene is 95.6%; When adsorption time was 600min, the separation rate of p-Nitrophenyl chloride was 98.6%.The separation rate of o-Nitrochlorobenzene is 95.8%.
Embodiment 3: with the o-Nitrochlorobenzene starting point concentration among the embodiment 1: the p-Nitrophenyl chloride starting point concentration is to change 2: 1 at 1: 1, and other operational condition remains unchanged, and the separation rate of p-Nitrophenyl chloride and o-Nitrochlorobenzene is constant substantially.
Embodiment 4: among the embodiment 1, other condition is constant, when temperature is got 278K; Adsorption time is 30min, and the separation rate of p-Nitrophenyl chloride is 99.6%, and the separation rate of o-Nitrochlorobenzene is 94.5%; When temperature was got 323K, the separation rate of p-Nitrophenyl chloride was 98.1%, and the separation rate of o-Nitrochlorobenzene is 94%.
Embodiment 5: with the contactor among the embodiment 1 is opening, adopts the constant temperature cradle vibrate, and the vibration rotating speed is 150 rev/mins, and other operational condition remains unchanged, and the separation rate of p-Nitrophenyl chloride and o-Nitrochlorobenzene is constant substantially.
Embodiment 6: the weisspiessglanz among the embodiment 1 is accounted for 16% of the preceding mixture total mass of calcining, be about 0.027g; The HZSM-5 zeolite granular diameter that weisspiessglanz is modified is 1.5 μ m; The vibration rotating speed is 60 rev/mins; The o-Nitrochlorobenzene starting point concentration: the p-Nitrophenyl chloride starting point concentration is 4: 1; When adsorption time was 900min, other condition was constant, and the rate of recovery of p-Nitrophenyl chloride is 93.2%, and the separation rate of o-Nitrochlorobenzene is 94%.
Embodiment 7: weisspiessglanz accounts for 8% of the preceding mixture total mass of calcining among the embodiment 1, is about 0.014g; The HZSM-5 zeolite granular diameter that weisspiessglanz is modified is 18 μ m; The vibration rotating speed is 190 rev/mins; The o-Nitrochlorobenzene starting point concentration: the p-Nitrophenyl chloride starting point concentration is 5: 1, and other condition is constant, and the rate of recovery of p-Nitrophenyl chloride is 91.4%, and the separation rate of o-Nitrochlorobenzene is 93.5%.
Embodiment 8: change the eluting temperature among the embodiment 1 into 320K, other operational condition remains unchanged, and the nitro-chlorobenzene rate of recovery reaches 100%; Eluting temperature changes 278K into, and the nitro-chlorobenzene rate of recovery reaches 99%.
Embodiment 9: change the elutriant among the embodiment 1 into methyl alcohol, other operational condition remains unchanged, and the rate of recovery of nitro-chlorobenzene is 89%; Elutriant changes acetone into, and the rate of recovery of nitro-chlorobenzene is 27%.
Claims (6)
1, a kind of HZSM-5 zeolite adsorption of weisspiessglanz modification is divided clutch nitro-chlorobenzene waste water and resource recycling method, it is characterized in that, the contactor that the organic waste water that contains the nitro-chlorobenzene isomer that will handle is delivered to the HZSM-5 zeolite that the weisspiessglanz modification is housed adsorbs, and its condition is: the HZSM-5 zeolite granular diameter that weisspiessglanz is modified is 0.5～20 μ m; Weisspiessglanz accounts for 5%～20% of the preceding mixed powder quality of calcining; Nitro-chlorobenzene ortho isomer and the para-isomeride starting point concentration ratio in waste water is 1～5: 1; The vibration rotating speed is 50～200 rev/mins; Temperature range is 275～340K; Adsorption time is 10s～12h.
2, method according to claim 1 is characterized in that weisspiessglanz accounts for 20% of the preceding mixture total mass of calcining; Adopt magnetic agitation, the vibration rotating speed is 100～150 rev/mins; The o-Nitrochlorobenzene starting point concentration: the p-Nitrophenyl chloride starting point concentration is 1～2: 1; Temperature is got 278～323K; Adsorption time is 10s～30min.
3, method according to claim 1 is characterized in that need carrying out some conventional pre-treatment before the nitro-chlorobenzene waste water of handling enters contactor.
4, method according to claim 1 is characterized in that stirring and adopts the constant temperature cradle vibrate, or adopts constant temperature magnetic force device to stir.
5, method according to claim 1, it is characterized in that contactor be sealing or opening.
6, method according to claim 1 is characterized in that the desorbing agent of nitro-chlorobenzene is selected methyl alcohol or ethanol organic solvent for use.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410014258.3A CN1234617C (en) | 2004-03-10 | 2004-03-10 | Process for adsorpting and separating waste water containing nitro-chlrobenzene by antimony oxide modified zeloite and resource recovery process thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200410014258.3A CN1234617C (en) | 2004-03-10 | 2004-03-10 | Process for adsorpting and separating waste water containing nitro-chlrobenzene by antimony oxide modified zeloite and resource recovery process thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1559922A true CN1559922A (en) | 2005-01-05 |
| CN1234617C CN1234617C (en) | 2006-01-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200410014258.3A Expired - Fee Related CN1234617C (en) | 2004-03-10 | 2004-03-10 | Process for adsorpting and separating waste water containing nitro-chlrobenzene by antimony oxide modified zeloite and resource recovery process thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100497174C (en) * | 2005-04-21 | 2009-06-10 | 中国石油化工股份有限公司 | Synthesis of zeolite molecular sieves |
| CN102872837A (en) * | 2012-09-04 | 2013-01-16 | 常州大学 | Composite adsorption material for removing strontium ions from natural water and preparation method for adsorption material |
-
2004
- 2004-03-10 CN CN200410014258.3A patent/CN1234617C/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100497174C (en) * | 2005-04-21 | 2009-06-10 | 中国石油化工股份有限公司 | Synthesis of zeolite molecular sieves |
| CN102872837A (en) * | 2012-09-04 | 2013-01-16 | 常州大学 | Composite adsorption material for removing strontium ions from natural water and preparation method for adsorption material |
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| Publication number | Publication date |
|---|---|
| CN1234617C (en) | 2006-01-04 |
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